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HRID1606489

反应详情

EQUATION

反应方程式

HRID 1606489 的结构方程式

REACTANTS

反应物

2
结构：Cc1ccc(S(=O)(=O)O)cc1
HCID6101

4-Methylbenzenesulfonic acid

C7H8O3S

结构：C[C@@H]1C[C@@]2(C)[C@@H](CC[C@H]3[C@@H]4CC[C@H](C5(C)OCCO5)[C@@]4(C)CC(=O)[C@@H]32)C[C@@H]1O
HCID70585127

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@H](O)[C@H](C)C[C@]4(C)[C@H]3C(=O)C[C@]12C
HCID86733333

未命名化合物

收率 51.9%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)=O
溶剂HCID180

Acetone

C3H6O

PROCEDURE

实验过程

A solution of 20,20-ethylenedioxy-3α-hydroxy-2α-methyl-5α-pregnane-11-one (0.38 g.) and toluene-p-sulphonic acid (30 mg.) in acetone (20 ml.) was kept at room temperature for 11/2 hr. The reaction mixture was then evaporated to low bulk and an aqueous solution of sodium hydrogen carbonate was added. The precipitated solid (0.32 g.) was collected and purified by preparative t.l.c. and crystallised from methyl acetate/petrol (b.p. 60°-80°) to give the title compound (0.175 g.), m.p. 179°-180°, [α]D + 125°.

WORKUP

后处理

  1. customwas kept at room temperature for 11
  2. custom2 hr
  3. customThe reaction mixture was then evaporated to low bulk
  4. additionan aqueous solution of sodium hydrogen carbonate was added
  5. customThe precipitated solid (0.32 g.) was collected
  6. custompurified by preparative t.l.c
  7. customand crystallised from methyl acetate/petrol (b.p. 60°-80°)