HRID2056096

反应详情

EQUATION

反应方程式

HRID 2056096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a mixture of tert-butyl 3-(4-amino-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-1-piperidinecarboxylate (1.2 g, 0.0027 mol) in acetone (20 mL) was added an aqueous 6N solution of hydrogen chloride (8 mL) at room temperature. The mixture was stirred at 45° C. for 1.5 hours, and then room temperature for 16 hours. The precipitate was filtered and washed with acetone. The solid was dried to give 3-iodo-1-(3-piperidyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine dihydrochloride (1 g, 0.0024 mol). TLC (methanol/dichloromethane=5:95) Rf 0.14 MS: MH+ 345

WORKUP

后处理

  1. waitroom temperature for 16 hours
  2. filtrationThe precipitate was filtered
  3. washwashed with acetone
  4. customThe solid was dried