huagongshe.com
HRID371826

反应详情

EQUATION

反应方程式

HRID 371826 的结构方程式

REACTANTS

反应物

3
结构：c1ccncc1
HCID1049

Pyridine

C5H5N

结构：CC(C)(C)[Si](C)(C)Cl
HCID28928

Chloro(1,1-dimethylethyl)dimethylsilane

C6H15ClSi

结构：C[C@]12CC[C@H]3[C@@H](CCC4=CC(=O)CC[C@@]43CO)[C@@H]1CCC2=O
HCID252379

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)[Si](C)(C)OC[C@]12CCC(=O)C=C1CC[C@@H]1[C@@H]2CC[C@]2(C)C(=O)CC[C@@H]12
HCID10573974

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

19-Hydroxy-4-androstene-3,17-dione, t-butyldimethylsilylchloride and pyridine are mixed in dry dimethylformamide and heated on a steam bath overnight. The reaction mixture is poured onto water and stirred well for 15 minutes. The resulting solid is filtered and dissolved in methylenechloride, dried over magnesium sulfate and the solvent removed. The residue is crystallized from an acetone-hexane solution to yield 19-t-butyldimethylsiloxy-4-androstene-3,17-dione.

WORKUP

后处理

  1. temperatureheated on a steam bath overnight
  2. additionThe reaction mixture is poured onto water
  3. filtrationThe resulting solid is filtered
  4. dissolutiondissolved in methylenechloride
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent removed
  7. customThe residue is crystallized from an acetone-hexane solution