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HRID1912696

反应详情

EQUATION

反应方程式

HRID 1912696 的结构方程式

REACTANTS

反应物

2
结构：C[C@]12CCCCC1C(=O)C[C@@H]1[C@@H]2CC[C@@]2(C)[C@H]1CC13OCCOC12OCCO3
HCID67535914

未命名化合物

结构：C=C1C[C@@H]2[C@H](CC[C@@]3(C)[C@H]2CC24OCCOC23OCCO4)[C@@]2(C)CCCCC12
HCID67535939

未命名化合物

PRODUCTS

生成物

1
结构：C/C=C1\C[C@@H]2[C@H](CC[C@@]3(C)[C@H]2CC24OCCOC23OCCO4)[C@@]2(C)CCCCC12
HCID86651505

未命名化合物

收率 96%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
催化剂HCID73727

Phosphonium, ethyltriphenyl-, bromide (1:1)

C20H20BrP

PROCEDURE

实验过程

17,17-Bis(ethylendioxy)-6(E)-ethylidenandrostane was prepared in 96% yield from 3,3:17,17-bis(ethylendioxy)androstane-6-one and (ethyl)triphenylphosphonium bromide by the procedure described above for the preparation of 3,3:17,17-bis(ethylendioxy)-6-methyleneandrostane (Prepn. 8). The mixture was purified by flash chromatography (SiO2, cyclohexane/EtOAc 85/15). 1H-NMR (300 MHz, acetone-d6, ppm from TMS): δ 4.91 (m, 1H), 3.93-3.78 (m, 8H), 2.69 (m, 1H), 2.10-0.85 (m, 22H), 0.81 (s, 3H), 0.66 (s, 3H).

WORKUP

后处理

  1. customThe mixture was purified by flash chromatography (SiO2, cyclohexane/EtOAc 85/15)