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HRID361654

反应详情

EQUATION

反应方程式

HRID 361654 的结构方程式

REACTANTS

反应物

2
结构：O=S(=O)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
HCID67814

Perfluorobutanesulfonyl fluoride

C4F10O2S

结构：C[C@]12C[C@@H](O)[C@H]3[C@@H](CCC4=CC(=O)CC[C@@H]43)[C@@H]1CCC2=O
HCID10902298

11alpha-Hydroxy-estr-4-ene-3,17-dione

C18H24O3

PRODUCTS

生成物

1
结构：C[C@]12C[C@H](F)[C@H]3[C@@H](CCC4=CC(=O)CC[C@@H]43)[C@@H]1CCC2=O
HCID10979145

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

3
结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

结构：C1CCC2=NCCCN2CC1
溶剂HCID81184

1,8-Diazabicyclo[5.4.0]undec-7-ene

C9H16N2

PROCEDURE

实验过程

4.6 ml of perfluorobutane-1-sulfonic acid fluoride is added in drops to 5.0 g of 11α-hydroxy-estr-4-ene-3,17-dione in 100 ml of toluene and 7.3 ml of 1,8-diazabicyclo[5,4,0]undec-7-ene at 0° C. After 30 minutes, the solution is diluted with ethyl acetate, washed with saturated sodium chloride solution, dried and concentrated by evaporation in a vacuum. After the crude product is chromatographed on silica gel with a hexane-ethyl acetate gradient, 3.8 g of 11β-fluoro-estr-4-ene-3,17-dione with a melting point of 173°-174° C. is obtained.

WORKUP

后处理

  1. washwashed with saturated sodium chloride solution
  2. customdried
  3. concentrationconcentrated by evaporation in a vacuum
  4. customAfter the crude product is chromatographed on silica gel with a hexane-ethyl acetate gradient, 3.8 g of 11β-fluoro-estr-4-ene-3,17-dione with a melting point of 173°-174° C.
  5. customis obtained