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HRID259156

反应详情

EQUATION

反应方程式

HRID 259156 的结构方程式

REACTANTS

反应物

3
结构：CN(C)C=O
HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CC(=O)[O-].[K+]
HCID517044

Potassium acetate

C2H3KO2

结构：CC(=O)OCC(=O)[C@@]1(OC(C)=O)CC[C@H]2[C@@H]3CC[C@H]4CC(=O)CC[C@]4(C)[C@@]3(F)[C@@H](O[Si](C)(C)C)C[C@@]21C
HCID22798521

11beta-Trimethylsiloxy-17alpha,21-diacetoxy9alphafluoro-5alpha-pregnane3,20-dione

C28H43FO7Si

PRODUCTS

生成物

1
结构：CC(=O)OCC(=O)C1=CC[C@H]2[C@@H]3CC[C@H]4CC(=O)CC[C@]4(C)[C@@]3(F)[C@@H](O[Si](C)(C)C)C[C@]12C
HCID22798533

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

PROCEDURE

实验过程

A mixture of 8.0 g of 11β-trimethylsiloxy-17α,21-diacetoxy9αfluoro-5α-pregnane3,20-dione obtained according to Example 19, 4 g anhydrous potassium acetate and 20 ml of dimethyl formamide was heated for a period of 4 hours at 110° -120° in an atmosphere of nitrogen. The reaction mixture was cooled and poured into 120 ml of water and ice. The mixture was left stirring for 30 minutes, then lft standing for a period of 2 hours, filtered, washed on the filter with abundant water, collected and dried. Trituration of this crude product with acetone/ether gave 11β-trimethylsiloxy-21-acetoxy-9α-fluoro-5α-pregn-16-ene-3,20-dione (compound 44). Yield: 7.0 g.

WORKUP

后处理

  1. customobtained
  2. temperaturewas heated for a period of 4 hours at 110° -120° in an atmosphere of nitrogen
  3. temperatureThe reaction mixture was cooled
  4. waitThe mixture was left
  5. waitlft standing for a period of 2 hours
  6. filtrationfiltered
  7. washwashed on the
  8. filtrationfilter with abundant water
  9. customcollected
  10. customdried