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HRID918374

反应详情

EQUATION

反应方程式

HRID 918374 的结构方程式

REACTANTS

反应物

3
结构：CCOC(CNC(N)=O)OCC
HCID1713901

Urea, (2,2-diethoxyethyl)-

C7H16N2O3

结构：CCOC(C=[N+]=[N-])OCC
HCID21520892

Ethane, 2-diazo-1,1-diethoxy-

C6H12N2O2

结构：C[C@]12C=CC(=O)C=C1CC[C@H]1[C@@H]3C[C@@H](O)[C@](O)(C(=O)CCl)[C@@]3(C)C[C@H](O)[C@@]12F
HCID86733740

未命名化合物

PRODUCTS

生成物

1
结构：CCOC(CO[C@@H]1C[C@H]2[C@@H]3CCC4=CC(=O)C=C[C@]4(C)[C@@]3(F)[C@@H](O)C[C@]2(C)[C@@]1(O)C(=O)CCl)OCC
HCID86733742

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 2,2-diethoxy-1-diazoethane (prepared from 0.0935 mole of N-2,2-diethoxyethyl urea by the method of W. Kirmse and M. Buschhoff, Chem. Ber., 100, 1491 (1967)) in 300 ml of 3:2 ether-pentane is diluted with 100 ml of methanol and cooled to 0°C. A total of 2.5 g of 21-chloro-9-fluoro-11β,16α,17-trihydroxypregna-1,4-diene-3,20-dione, 16,17-cycloborate is added in portions until nitrogen evolution ceases. The solvent is removed in vacuo and the residue is dissolved in chloroform and chromatographed on an 80 g -- silica gel column. Elution with chloroform gives 2.16 g of TLC pure material that is recrystallized from acetone-hexane to give 1.75 g of 21-chloro-16α-(2,2-diethoxyethoxy)-9-fluoro-11β,17-dihydroxypregna-1,4-diene-3,20-dione, melting point 200°-202°C.

WORKUP

后处理

  1. customThe solvent is removed in vacuo
  2. dissolutionthe residue is dissolved in chloroform
  3. customchromatographed on an 80 g
  4. washElution with chloroform
  5. customgives 2.16 g of TLC pure material that
  6. customis recrystallized from acetone-hexane