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HRID1838881

反应详情

EQUATION

反应方程式

HRID 1838881 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：CC(=O)OC(C)=O
HCID7918

Acetic anhydride

C4H6O3

结构：C[C@]12C[C@H](F)[C@H]3[C@@H]([C@H](CCCCCO)CC4=CC(=O)CC[C@@H]43)[C@@H]1CCC2=O
HCID15870661

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)OCCCCC[C@@H]1CC2=CC(=O)CC[C@@H]2[C@@H]2[C@@H]1[C@@H]1CCC(=O)[C@@]1(C)C[C@@H]2F
HCID69935327

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：c1ccncc1
溶剂HCID1049

Pyridine

C5H5N

PROCEDURE

实验过程

20 g of 11β-fluoro-7α-(5-hydroxypentyl)oestr-4-ene-3,17-dione in 100 ml of pyridine are allowed to react at 25° C. for 2 h with 50 ml of acetic anhydride. 5 ml of water are then added at 0° C. and the mixture is stirred for 45 min. It is extracted with diethyl ether, washed with 2N sulphuric acid until free of pyridine and neutralized successively with saturated sodium hydrogencarbonate solution and water. After drying and concentrating in vacuo, the crude product is chromatographed on silica gel using a hexane-ethyl acetate gradient. 17 g of 7α-(5-acetoxypentyl)-11β-fluorooestr-4-ene-3,17-dione of melting point 78.4° C. are obtained.

WORKUP

后处理

  1. extractionIt is extracted with diethyl ether
  2. washwashed with 2N sulphuric acid until free of pyridine
  3. customAfter drying
  4. concentrationconcentrating in vacuo
  5. customthe crude product is chromatographed on silica gel using a hexane-ethyl acetate gradient