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HRID232809

反应详情

EQUATION

反应方程式

HRID 232809 的结构方程式

REACTANTS

反应物

4
结构：O=S(=O)(O)O
HCID1118

Sulfuric acid

H2O4S

结构：CCOCC
HCID3283

Diethyl Ether

C4H10O

结构：O=C([O-])O.[Na+]
HCID516892

Sodium Bicarbonate

CHNaO3

结构：CC(=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@@H]5O[C@@H]5C[C@]4(C)[C@H]3CC[C@]12C
HCID54346631

未命名化合物

PRODUCTS

生成物

1
结构：CO[C@H]1C[C@@]2(C)[C@@H](CC[C@@H]3[C@@H]2CC[C@]2(C)[C@@H](C(C)=O)CC[C@@H]32)C[C@@H]1O
HCID70086536

未命名化合物

收率 60%

AUXILIARIES

试剂、催化剂与溶剂

3
结构：CO
催化剂HCID887

Methanol

CH4O

结构：CO
溶剂HCID887

Methanol

CH4O

结构：CCCCCC.CCOC(C)=O
溶剂HCID21226206

未命名化合物

PROCEDURE

实验过程

2α,3α-Epoxy-5α-pregnan-20-one (325 mg) in 80 mL of methanol was treated with a 1 mL solution of methanol containing 7 drops of concentrated sulfuric acid at room temperature. This mixture was stirred at this temperature for 10 minutes and then poured into a cold saturated solution of sodium bicarbonate and ether. The organic phase was washed several times with a small portion of bicarbonate, brine and dried over potassium carbonate. The concentrated organic phase was tested by TLC for complete reaction. Flash chromatography on silica gel with hexane/ethyl acetate solvent mixture (80:20) produced 209 mg (60% yield).

WORKUP

后处理

  1. washThe organic phase was washed several times with a small portion of bicarbonate, brine
  2. dry with materialdried over potassium carbonate
  3. customThe concentrated organic phase was tested by TLC for complete reaction