HRID82144

反应详情

EQUATION

反应方程式

HRID 82144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Palladium (10% on carbon, 18 g) was added to 7-[(1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethyl]-4-chloro-7H-pyrrolo[2,3-d]pyrimidine (182 g, 558 mmol) (see Preparation 1) in ethanol (900 mL) and concentrated ammonia solution (100 mL) and hydrogenated (60 psi, 20° C.) for 18 hours. The reaction mixture was filtered through Arbocel™ and the filtrate was evaporated in vacuo. Diethyl ether (300 mL) was added to the residue and the mixture was filtered. The filtrate was evaporated in vacuo to afford the title compound as an orange oil in 94% yield, 162.7 g.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Arbocel™
  2. customthe filtrate was evaporated in vacuo
  3. additionDiethyl ether (300 mL) was added to the residue
  4. filtrationthe mixture was filtered
  5. customThe filtrate was evaporated in vacuo