The relative configuration was determined for the title compound, C26H34O6, which was prepared in a synthetic study on immunosuppressant FR65814. There is an intramolecular hydrogen bond between the hydroxy and epoxy groups.
Supporting information
CCDC reference: 145659
The title compound was synthesized from D-glucose (Amano et al., 1999). The stereochemistries at C-3 and C-4 (atom labels C3 and C4, respectively) came from those at C-2 and C-3 of D-glucose, respectively.
The positional parameters of all the H atoms were calculated geometrically and fixed with U(H) = 1.2Ueq(parent atom). The absolute structure was assigned based on the known absolute configurations around the C3 and C4 atoms, which came from D-glucose.
Data collection: MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.
Crystal data top
C26H34O6 | Dx = 1.209 Mg m−3 |
Mr = 442.55 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 25 reflections |
Hall symbol: P 2ac 2ab | θ = 10–15° |
a = 18.060 (3) Å | µ = 0.09 mm−1 |
b = 23.477 (3) Å | T = 296 K |
c = 5.736 (2) Å | Prism, colourless |
V = 2431 (1) Å3 | 0.6 × 0.4 × 0.4 mm |
Z = 4 | |
Data collection top
Rigaku AFC-5S diffractometer | θmax = 25° |
θ–2θ scans | h = 0→21 |
2493 measured reflections | k = 0→28 |
2493 independent reflections | l = 0→7 |
1281 reflections with I > 2σ(I) | 3 standard reflections every 100 reflections |
Rint = 0 | intensity decay: none |
Refinement top
Refinement on F2 | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.073 | w = 1/[σ2(Fo2) + {0.05(Fo2 + 2Fc2)/3}2] |
wR(F2) = 0.221 | (Δ/σ)max = 0.010 |
S = 1.92 | Δρmax = 0.21 e Å−3 |
2493 reflections | Δρmin = −0.19 e Å−3 |
292 parameters | Absolute structure: see text, no Friedel pairs |
Crystal data top
C26H34O6 | V = 2431 (1) Å3 |
Mr = 442.55 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 18.060 (3) Å | µ = 0.09 mm−1 |
b = 23.477 (3) Å | T = 296 K |
c = 5.736 (2) Å | 0.6 × 0.4 × 0.4 mm |
Data collection top
Rigaku AFC-5S diffractometer | Rint = 0 |
2493 measured reflections | 3 standard reflections every 100 reflections |
2493 independent reflections | intensity decay: none |
1281 reflections with I > 2σ(I) | |
Refinement top
R[F2 > 2σ(F2)] = 0.073 | H-atom parameters not refined |
wR(F2) = 0.221 | Δρmax = 0.21 e Å−3 |
S = 1.92 | Δρmin = −0.19 e Å−3 |
2493 reflections | Absolute structure: see text, no Friedel pairs |
292 parameters | |
Special details top
Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
O1 | −0.9626 (3) | −0.3139 (2) | −1.1771 (7) | 0.094 (2) | |
O2 | −0.8426 (3) | −0.2499 (2) | −1.2545 (7) | 0.096 (1) | |
O3 | −0.9397 (2) | −0.1625 (1) | −0.7384 (6) | 0.065 (1) | |
O4 | −0.8297 (2) | 0.0731 (2) | −0.3631 (10) | 0.110 (2) | |
O5 | −1.0898 (2) | −0.1989 (2) | −0.6585 (7) | 0.078 (1) | |
O6 | −1.3556 (3) | −0.0363 (2) | −0.355 (1) | 0.151 (3) | |
C1 | −0.9335 (4) | −0.3146 (3) | −0.945 (1) | 0.078 (2) | |
C2 | −0.9067 (3) | −0.2553 (2) | −0.8673 (9) | 0.060 (1) | |
C3 | −0.9710 (3) | −0.2142 (2) | −0.8387 (10) | 0.060 (1) | |
C4 | −1.0301 (3) | −0.2383 (2) | −0.6780 (10) | 0.068 (2) | |
C5 | −1.0576 (3) | −0.2938 (3) | −0.766 (1) | 0.087 (2) | |
C6 | −0.9948 (4) | −0.3375 (3) | −0.787 (1) | 0.091 (2) | |
C7 | −0.8425 (3) | −0.2344 (3) | −1.010 (1) | 0.071 (2) | |
C8 | −0.8526 (3) | −0.1918 (3) | −1.200 (1) | 0.083 (2) | |
C9 | −0.7952 (4) | −0.1503 (4) | −1.278 (1) | 0.122 (3) | |
C10 | −0.7688 (3) | −0.2426 (4) | −0.898 (1) | 0.118 (3) | |
C11 | −0.9723 (3) | −0.1107 (2) | −0.821 (1) | 0.081 (2) | |
C12 | −0.9355 (3) | −0.0630 (2) | −0.696 (1) | 0.076 (2) | |
C13 | −0.8669 (4) | −0.0438 (3) | −0.756 (1) | 0.093 (2) | |
C14 | −0.8318 (4) | 0.0014 (3) | −0.640 (2) | 0.105 (3) | |
C15 | −0.8666 (4) | 0.0281 (3) | −0.462 (1) | 0.088 (2) | |
C16 | −0.9358 (4) | 0.0098 (3) | −0.393 (1) | 0.107 (3) | |
C17 | −0.9685 (4) | −0.0362 (3) | −0.508 (1) | 0.105 (3) | |
C18 | −0.8662 (5) | 0.1021 (3) | −0.173 (2) | 0.126 (3) | |
C19 | −1.1092 (4) | −0.1854 (3) | −0.433 (1) | 0.098 (2) | |
C20 | −1.1727 (4) | −0.1431 (3) | −0.424 (1) | 0.081 (2) | |
C21 | −1.2256 (3) | −0.1431 (3) | −0.593 (1) | 0.093 (2) | |
C22 | −1.2874 (4) | −0.1058 (3) | −0.576 (1) | 0.091 (2) | |
C23 | −1.2947 (4) | −0.0730 (3) | −0.389 (1) | 0.093 (2) | |
C24 | −1.2427 (4) | −0.0730 (3) | −0.226 (1) | 0.104 (3) | |
C25 | −1.1814 (4) | −0.1068 (3) | −0.239 (1) | 0.101 (3) | |
C26 | −1.4026 (5) | −0.0300 (6) | −0.527 (3) | 0.215 (6) | |
H1 | −0.924 | −0.289 | −1.23 | 0.1263* | |
H2 | −0.8923 | −0.3405 | −0.9403 | 0.0938* | |
H3 | −0.8872 | −0.2607 | −0.7132 | 0.0724* | |
H4 | −0.9923 | −0.2058 | −0.9883 | 0.0725* | |
H5 | −1.0088 | −0.2440 | −0.5263 | 0.0819* | |
H6 | −1.0944 | −0.3082 | −0.6606 | 0.1048* | |
H7 | −1.0795 | −0.2882 | −0.9172 | 0.1048* | |
H8 | −1.0140 | −0.3722 | −0.8523 | 0.1093* | |
H9 | −0.9748 | −0.3450 | −0.6353 | 0.1093* | |
H10 | −0.9026 | −0.1786 | −1.2177 | 0.0994* | |
H11 | −0.7484 | −0.1603 | −1.2100 | 0.1461* | |
H12 | −0.7914 | −0.1513 | −1.4444 | 0.1461* | |
H13 | −0.8090 | −0.1127 | −1.2282 | 0.1461* | |
H14 | −0.7548 | −0.2819 | −0.9086 | 0.1411* | |
H15 | −0.7326 | −0.2196 | −0.9765 | 0.1411* | |
H16 | −0.7716 | −0.2315 | −0.7373 | 0.1411* | |
H17 | −0.9646 | −0.1070 | −0.9858 | 0.0977* | |
H18 | −1.0244 | −0.1105 | −0.7883 | 0.0977* | |
H19 | −0.8415 | −0.0620 | −0.8830 | 0.1116* | |
H20 | −0.7831 | 0.0133 | −0.6861 | 0.1254* | |
H21 | −0.9612 | 0.0284 | −0.2675 | 0.1280* | |
H22 | −1.0157 | −0.0498 | −0.4547 | 0.1258* | |
H23 | −0.8353 | 0.1326 | −0.1182 | 0.1515* | |
H24 | −0.9125 | 0.1174 | −0.2263 | 0.1515* | |
H25 | −0.8750 | 0.0758 | −0.0481 | 0.1515* | |
H26 | −1.1238 | −0.2196 | −0.3539 | 0.1176* | |
H27 | −1.0670 | −0.1691 | −0.3563 | 0.1176* | |
H28 | −1.2211 | −0.1682 | −0.7244 | 0.1115* | |
H29 | −1.3235 | −0.1043 | −0.6987 | 0.1087* | |
H30 | −1.2484 | −0.0482 | −0.0940 | 0.1250* | |
H31 | −1.1446 | −0.1052 | −0.1182 | 0.1215* | |
H32 | −1.4410 | −0.0041 | −0.4810 | 0.2581* | |
H33 | −1.3772 | −0.0151 | −0.6608 | 0.2581* | |
H34 | −1.4240 | −0.0663 | −0.5655 | 0.2581* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
O1 | 0.123 (4) | 0.094 (3) | 0.064 (3) | −0.006 (3) | −0.037 (3) | −0.009 (3) |
O2 | 0.118 (3) | 0.106 (3) | 0.063 (2) | 0.007 (3) | 0.010 (3) | −0.013 (3) |
O3 | 0.067 (2) | 0.065 (2) | 0.065 (2) | 0.010 (2) | −0.011 (2) | −0.012 (2) |
O4 | 0.099 (3) | 0.092 (3) | 0.140 (5) | −0.013 (3) | −0.012 (3) | −0.034 (3) |
O5 | 0.064 (2) | 0.105 (3) | 0.066 (2) | 0.016 (2) | −0.002 (2) | 0.004 (2) |
O6 | 0.103 (4) | 0.146 (5) | 0.203 (7) | 0.037 (3) | 0.015 (4) | 0.039 (5) |
C1 | 0.100 (4) | 0.071 (3) | 0.063 (3) | 0.011 (3) | −0.024 (3) | −0.016 (3) |
C2 | 0.077 (3) | 0.061 (3) | 0.044 (3) | 0.016 (2) | −0.012 (3) | −0.001 (3) |
C3 | 0.059 (3) | 0.066 (3) | 0.056 (3) | 0.001 (2) | −0.013 (2) | 0.003 (3) |
C4 | 0.068 (3) | 0.079 (3) | 0.058 (3) | 0.002 (2) | −0.005 (3) | 0.014 (3) |
C5 | 0.094 (4) | 0.082 (3) | 0.086 (4) | −0.024 (3) | −0.009 (5) | 0.012 (4) |
C6 | 0.115 (4) | 0.077 (4) | 0.081 (5) | −0.008 (3) | −0.018 (4) | 0.017 (4) |
C7 | 0.066 (3) | 0.083 (4) | 0.063 (2) | 0.021 (3) | −0.006 (2) | −0.006 (2) |
C8 | 0.086 (4) | 0.105 (3) | 0.058 (4) | 0.024 (3) | 0.005 (4) | 0.002 (3) |
C9 | 0.105 (5) | 0.160 (7) | 0.100 (6) | −0.022 (4) | 0.045 (5) | 0.022 (6) |
C10 | 0.068 (4) | 0.180 (7) | 0.104 (6) | 0.021 (5) | −0.018 (4) | 0.031 (6) |
C11 | 0.093 (4) | 0.064 (3) | 0.088 (5) | 0.011 (3) | −0.027 (4) | 0.001 (3) |
C12 | 0.076 (3) | 0.053 (3) | 0.099 (5) | 0.015 (3) | −0.013 (3) | 0.003 (3) |
C13 | 0.081 (4) | 0.097 (5) | 0.101 (5) | 0.006 (3) | 0.019 (4) | −0.027 (4) |
C14 | 0.077 (4) | 0.106 (5) | 0.131 (7) | −0.009 (4) | 0.018 (4) | −0.033 (4) |
C15 | 0.089 (4) | 0.068 (4) | 0.108 (5) | 0.012 (3) | −0.013 (3) | −0.002 (3) |
C16 | 0.102 (4) | 0.114 (5) | 0.104 (6) | −0.014 (4) | 0.031 (5) | −0.051 (5) |
C17 | 0.087 (5) | 0.112 (5) | 0.115 (6) | −0.014 (4) | 0.021 (4) | −0.041 (4) |
C18 | 0.147 (7) | 0.108 (6) | 0.123 (7) | 0.009 (5) | −0.026 (5) | −0.047 (5) |
C19 | 0.093 (5) | 0.130 (6) | 0.072 (3) | 0.037 (4) | 0.016 (4) | 0.010 (4) |
C20 | 0.071 (4) | 0.107 (5) | 0.066 (4) | −0.001 (3) | 0.012 (3) | 0.017 (3) |
C21 | 0.084 (4) | 0.119 (5) | 0.076 (4) | 0.013 (3) | −0.008 (3) | −0.009 (5) |
C22 | 0.081 (4) | 0.111 (6) | 0.080 (5) | 0.009 (3) | −0.027 (4) | 0.004 (4) |
C23 | 0.092 (4) | 0.100 (5) | 0.088 (5) | −0.012 (3) | 0.011 (4) | 0.003 (4) |
C24 | 0.105 (5) | 0.118 (6) | 0.090 (5) | 0.009 (4) | 0.001 (4) | −0.031 (5) |
C25 | 0.093 (5) | 0.134 (6) | 0.077 (5) | 0.006 (4) | −0.010 (5) | −0.020 (4) |
C26 | 0.137 (8) | 0.27 (1) | 0.24 (1) | 0.092 (9) | −0.043 (8) | 0.01 (1) |
Geometric parameters (Å, º) top
O1—C1 | 1.429 (10) | C10—H15 | 0.960 |
O1—H1 | 0.960 | C10—H16 | 0.960 |
O2—C7 | 1.45 (1) | C11—C12 | 1.48 (1) |
O2—C8 | 1.411 (10) | C11—H17 | 0.960 |
O3—C3 | 1.457 (8) | C11—H18 | 0.960 |
O3—C11 | 1.431 (8) | C12—C13 | 1.36 (1) |
O4—C15 | 1.37 (1) | C12—C17 | 1.38 (1) |
O4—C18 | 1.45 (1) | C13—C14 | 1.41 (1) |
O5—C4 | 1.424 (8) | C13—H19 | 0.960 |
O5—C19 | 1.38 (1) | C14—C15 | 1.35 (1) |
O6—C23 | 1.41 (1) | C14—H20 | 0.960 |
O6—C26 | 1.31 (2) | C15—C16 | 1.38 (1) |
C1—C2 | 1.54 (1) | C16—C17 | 1.40 (1) |
C1—C6 | 1.53 (1) | C16—H21 | 0.960 |
C1—H2 | 0.960 | C17—H22 | 0.960 |
C2—C3 | 1.521 (10) | C18—H23 | 0.960 |
C2—C7 | 1.50 (1) | C18—H24 | 0.960 |
C2—H3 | 0.960 | C18—H25 | 0.960 |
C3—C4 | 1.519 (10) | C19—C20 | 1.52 (1) |
C3—H4 | 0.960 | C19—H26 | 0.960 |
C4—C5 | 1.48 (1) | C19—H27 | 0.960 |
C4—H5 | 0.960 | C20—C21 | 1.36 (1) |
C5—C6 | 1.53 (1) | C20—C25 | 1.37 (1) |
C5—H6 | 0.960 | C21—C22 | 1.42 (1) |
C5—H7 | 0.960 | C21—H28 | 0.960 |
C6—H8 | 0.960 | C22—C23 | 1.33 (1) |
C6—H9 | 0.960 | C22—H29 | 0.960 |
C7—C8 | 1.49 (1) | C23—C24 | 1.33 (1) |
C7—C10 | 1.49 (1) | C24—C25 | 1.36 (1) |
C8—C9 | 1.49 (1) | C24—H30 | 0.960 |
C8—H10 | 0.960 | C25—H31 | 0.960 |
C9—H11 | 0.960 | C26—H32 | 0.960 |
C9—H12 | 0.960 | C26—H33 | 0.960 |
C9—H13 | 0.960 | C26—H34 | 0.960 |
C10—H14 | 0.960 | | |
| | | |
O1···C4i | 3.590 (9) | O3···C8iii | 3.534 (10) |
O1···C6i | 3.59 (1) | C4···H1iii | 3.4 (1) |
O2···C21ii | 3.40 (1) | | |
| | | |
C1—O1—H1 | 90 | H14—C10—H15 | 109.5 |
C7—O2—C8 | 62.7 (5) | H14—C10—H16 | 109 |
C3—O3—C11 | 114.7 (5) | H15—C10—H16 | 109 |
C15—O4—C18 | 117.0 (8) | O3—C11—C12 | 107.3 (6) |
C4—O5—C19 | 114.6 (6) | O3—C11—H17 | 110.0 |
C23—O6—C26 | 118 (1) | O3—C11—H18 | 110.0 |
O1—C1—C2 | 112.0 (7) | C12—C11—H17 | 110.0 |
O1—C1—C6 | 106.8 (7) | C12—C11—H18 | 110.0 |
O1—C1—H2 | 108.7 | H17—C11—H18 | 109.5 |
C2—C1—C6 | 111.9 (7) | C11—C12—C13 | 122.4 (9) |
C2—C1—H2 | 108.7 | C11—C12—C17 | 121.7 (9) |
C6—C1—H2 | 108.7 | C13—C12—C17 | 115.9 (9) |
C1—C2—C3 | 111.5 (6) | C12—C13—C14 | 122.8 (9) |
C1—C2—C7 | 112.3 (7) | C12—C13—H19 | 118.6 |
C1—C2—H3 | 105.3 | C14—C13—H19 | 118.6 |
C3—C2—C7 | 116.1 (6) | C13—C14—C15 | 119.9 (9) |
C3—C2—H3 | 105.3 | C13—C14—H20 | 120 |
C7—C2—H3 | 105.3 | C15—C14—H20 | 120 |
O3—C3—C2 | 106.0 (5) | O4—C15—C14 | 116.3 (9) |
O3—C3—C4 | 110.1 (6) | O4—C15—C16 | 124.1 (10) |
O3—C3—H4 | 109.8 | C14—C15—C16 | 119.6 (10) |
C2—C3—C4 | 111.4 (6) | C15—C16—C17 | 119.2 (9) |
C2—C3—H4 | 109.8 | C15—C16—H21 | 120.4 |
C4—C3—H4 | 109.8 | C17—C16—H21 | 120.4 |
O5—C4—C3 | 109.7 (6) | C12—C17—C16 | 122.6 (9) |
O5—C4—C5 | 110.1 (6) | C12—C17—H22 | 118.7 |
O5—C4—H5 | 108.7 | C16—C17—H22 | 118.7 |
C3—C4—C5 | 110.8 (7) | O4—C18—H23 | 109 |
C3—C4—H5 | 108.7 | O4—C18—H24 | 109 |
C5—C4—H5 | 108.7 | O4—C18—H25 | 109.5 |
C4—C5—C6 | 111.5 (7) | H23—C18—H24 | 109.5 |
C4—C5—H6 | 109.0 | H23—C18—H25 | 109 |
C4—C5—H7 | 109.0 | H24—C18—H25 | 109 |
C6—C5—H6 | 109.0 | O5—C19—C20 | 112.1 (8) |
C6—C5—H7 | 109.0 | O5—C19—H26 | 108.8 |
H6—C5—H7 | 109.5 | O5—C19—H27 | 108.8 |
C1—C6—C5 | 110.3 (7) | C20—C19—H26 | 108.8 |
C1—C6—H8 | 109.3 | C20—C19—H27 | 108.8 |
C1—C6—H9 | 109.3 | H26—C19—H27 | 109.5 |
C5—C6—H8 | 109.3 | C19—C20—C21 | 120.3 (9) |
C5—C6—H9 | 109.3 | C19—C20—C25 | 121.4 (9) |
H8—C6—H9 | 109.5 | C21—C20—C25 | 118.2 (9) |
O2—C7—C2 | 116.4 (7) | C20—C21—C22 | 120.1 (9) |
O2—C7—C8 | 57.5 (5) | C20—C21—H28 | 120.0 |
O2—C7—C10 | 112.7 (8) | C22—C21—H28 | 120.0 |
C2—C7—C8 | 121.7 (7) | C21—C22—C23 | 119.4 (9) |
C2—C7—C10 | 114.2 (7) | C21—C22—H29 | 120 |
C8—C7—C10 | 120.8 (9) | C23—C22—H29 | 120 |
O2—C8—C7 | 59.8 (5) | O6—C23—C22 | 122 (1) |
O2—C8—C9 | 118.5 (7) | O6—C23—C24 | 117 (1) |
O2—C8—H10 | 114.2 | C22—C23—C24 | 120 (1) |
C7—C8—C9 | 124.9 (8) | C23—C24—C25 | 122 (1) |
C7—C8—H10 | 114.2 | C23—C24—H30 | 118 |
C9—C8—H10 | 114.2 | C25—C24—H30 | 118 |
C8—C9—H11 | 109.5 | C20—C25—C24 | 119.7 (10) |
C8—C9—H12 | 109.5 | C20—C25—H31 | 120 |
C8—C9—H13 | 109.5 | C24—C25—H31 | 120 |
H11—C9—H12 | 109.5 | O6—C26—H32 | 109 |
H11—C9—H13 | 109 | O6—C26—H33 | 109 |
H12—C9—H13 | 109 | O6—C26—H34 | 109 |
C7—C10—H14 | 109.5 | H32—C26—H33 | 109 |
C7—C10—H15 | 109.5 | H32—C26—H34 | 109 |
C7—C10—H16 | 109.5 | H33—C26—H34 | 109 |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y−1/2, −z−2; (iii) x, y, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O2 | 0.96 | 1.73 | 2.673 (9) | 166 |
Experimental details
Crystal data |
Chemical formula | C26H34O6 |
Mr | 442.55 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 296 |
a, b, c (Å) | 18.060 (3), 23.477 (3), 5.736 (2) |
V (Å3) | 2431 (1) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.09 |
Crystal size (mm) | 0.6 × 0.4 × 0.4 |
|
Data collection |
Diffractometer | Rigaku AFC-5S diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2493, 2493, 1281 |
Rint | 0 |
(sin θ/λ)max (Å−1) | 0.595 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.073, 0.221, 1.92 |
No. of reflections | 2493 |
No. of parameters | 292 |
No. of restraints | ? |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.21, −0.19 |
Absolute structure | See text, no Friedel pairs |
Selected geometric parameters (Å, º) topO1—C1 | 1.429 (10) | O3—C3 | 1.457 (8) |
O2—C7 | 1.45 (1) | O5—C4 | 1.424 (8) |
O2—C8 | 1.411 (10) | C7—C8 | 1.49 (1) |
| | | |
C7—O2—C8 | 62.7 (5) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O2 | 0.96 | 1.73 | 2.673 (9) | 166 |
The total synthesis of novel immunosuppressant FR65814 was reported (Amano et al., 1998, 1999). The title compound, (I), was prepared in a synthetic study on FR65814.