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HRID1837212

反应详情

EQUATION

反应方程式

HRID 1837212 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：CNCCCCC[C@@H]1Cc2cc(O)ccc2[C@@H]2[C@@H]1[C@@H]1CC[C@H](O)[C@@]1(C)C[C@@H]2F
HCID15858642

未命名化合物

结构：Cc1ccc(S(=O)(=O)[O-])c(CCCCCCCC(F)(F)C(F)(F)F)c1
HCID23497152

未命名化合物

PRODUCTS

生成物

1
结构：CN(CCCCCCCC(F)(F)C(F)(F)F)CCCCC[C@@H]1Cc2cc(O)ccc2[C@@H]2[C@@H]1[C@@H]1CC[C@H](O)[C@@]1(C)C[C@@H]2F
HCID15858644

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

PROCEDURE

实验过程

A solution of 1.77 g of 11β-fluoro-7α-[5-(methyl-amino)-pentyl]-estra-1,3,5(10)-triene-3,17β-diol in 18 ml of dimethylformamide is stirred with 1.4 g of 8,8,9,9,9-pentafluoro-nonyltosylate for 1 hour at a bath temperature of 80° C. Then, it is added to water, extracted three times with ethyl acetate, washed with water and common salt solution, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with dichloromethane/methanol. 11β-Fluoro-7α-{5-[methyl-(8,8,9,9,9-pentafluoro-nonyl)-amino]-pentyl}-estra-1,3,5(10)-triene-3,17β-diol is obtained as crystals with a melting point of 110° C.

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. washwashed with water and common salt solution
  3. customdried on sodium sulfate
  4. concentrationconcentrated by evaporation in a vacuum
  5. customchromatographed on silica gel with dichloromethane/methanol