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HRID900675

反应详情

EQUATION

反应方程式

HRID 900675 的结构方程式

REACTANTS

反应物

6
结构：CC1(C)C(=O)N(Br)C(=O)N1Br
HCID6479

1,3-Dibromo-5,5-dimethylhydantoin

C5H6Br2N2O2

结构：O=C([O-])[O-].[Li+].[Li+]
HCID11125

Lithium carbonate

CLi2O3

结构：O=S([O-])[O-].[Na+].[Na+]
HCID24437

Sodium sulfite

Na2O3S

结构：[Br-].[Li+]
HCID82050

Lithium bromide

BrLi

结构：CC(=O)[O-].[Na+]
HCID517045

Sodium Acetate

C2H3NaO2

结构：COC1=CC2=CC[C@@H]3[C@H]([C@@H](F)C[C@]4(C)C(=O)CC[C@@H]34)[C@H]2CC1
HCID11738260

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12C[C@H](F)[C@H]3[C@@H](C=CC4=CC(=O)CC[C@@H]43)[C@@H]1CCC2=O
HCID11173744

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

5 ml of a 10% by weight sodium acetate solution and, in portions, 2.5 g of 1,3-dibromo-5,5-dimethylhydantoin were added in succession at 0° C. to 5.0 g of 11β-fluoro-3-methoxy-estra-3,5-dien-17-one (A″) in 50 ml of DMF. After 30 minutes, 2.3 g of sodium sulfite and then 2.5 g of lithium bromide and 2.0 g of lithium carbonate were added and stirred for 2 hours at 100° C. The reaction mixture was stirred into ice water. The precipitated product was suctioned off, dissolved in ethyl acetate, washed with water, dried and concentrated by evaporation in a vacuum. After recrystallization from ethyl acetate, 3.6 g of 11β-fluoro-estra-4,6-diene-3,17-dione (B) with a melting point of 198° C. was obtained.

WORKUP

后处理

  1. washwashed with water
  2. customdried
  3. concentrationconcentrated by evaporation in a vacuum
  4. customAfter recrystallization from ethyl acetate, 3.6 g of 11β-fluoro-estra-4,6-diene-3,17-dione (B) with a melting point of 198° C.
  5. customwas obtained