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HRID1912708

反应详情

EQUATION

反应方程式

HRID 1912708 的结构方程式

REACTANTS

反应物

1
结构：C[C@]12CC[C@H](O)CC1CC(=O)[C@@H]1[C@@H]2CC[C@]2(C)C(=O)CC[C@@H]12
HCID69008093

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12CCC(=O)CC1CC(=O)[C@@H]1[C@@H]2CC[C@]2(C)C(=O)CC[C@@H]12
HCID24833691

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CCC[N+](CCC)(CCC)CCC.O=[Ru](=O)(=O)[O-]
催化剂HCID178419074

未命名化合物

结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

To a stirred solution of 3β-hydroxyandrostane-7,17-dione (1.65 g), TPAP (0.100 g), NMNO (1.40 g) under N2 in CH2Cl2 (90 mL), molecular sieve type 4 Å powder (2.6 g) was added. After 0.5 h the mixture was filtered and the filtrate was purified by flash chromatography (SiO2, CH2Cl2) to give the title compound II-bp (1.32 g, 81%). 1H-NMR (300 MHz, acetone-d6, ppm from TMS): δ 2.82-1.12 (m, 20H), 1.39 (s, 3H), 0.88 (s, 3H).

WORKUP

后处理

  1. filtrationAfter 0.5 h the mixture was filtered
  2. customthe filtrate was purified by flash chromatography (SiO2, CH2Cl2)