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HRID2397967

反应详情

EQUATION

反应方程式

HRID 2397967 的结构方程式

REACTANTS

反应物

2
结构：C[C@H]1CC(=O)C=C2CC[C@H]3[C@@H]4CC[C@H](O)[C@@]4(C)CC[C@@H]3[C@]21CO
HCID22797425

未命名化合物

结构：CC(C)=O.O=S(=O)(O)O.[O]=[Cr](=[O])=[O]
HCID131709961

未命名化合物

PRODUCTS

生成物

1
结构：C[C@H]1CC(=O)C=C2CC[C@@H]3[C@H](CC[C@]4(C)C(=O)CC[C@@H]34)[C@]21C=O
HCID54386542

未命名化合物

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

To a solution of 17β,19-dihydroxy-1α-methyl-4-androsten-3-one in acetone at 20° C. is added 2 equivalents of Jones Reagent with stirring. After 15 minutes the upper acetone layer is decanted and poured onto ice water and stirred for an additional 30 minutes. The precipitate which forms is filtered, washed with water and dissolved in ether. The ether solution is dried over magnesium sulfate and concentrated under reduced pressure. The residue is crystallized from acetone-hexane to yield 1α-methyl-4-androstene-3,17,19-trione.

WORKUP

后处理

  1. customAfter 15 minutes the upper acetone layer is decanted
  2. additionpoured onto ice water
  3. stirringstirred for an additional 30 minutes
  4. filtrationThe precipitate which forms is filtered
  5. washwashed with water
  6. dissolutiondissolved in ether
  7. dry with materialThe ether solution is dried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue is crystallized from acetone-hexane