HRID8294

反应详情

EQUATION

反应方程式

HRID 8294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A suspension of 4-(2-furyl)-1-(3-nitrobenzyl)-1H-pyrazolo[3,4-d]pyrimidine-6-amine (396 mg, 1.18 mmol) in EtOH (5 mL) was heated to 50° C., treated with a solution of SnCl2.2H2O (798 mg, 3.54 mmol) in conc. HCl (1.8 mL), stirred at 50° C. for 2 h then heated at 70° C. for 2 h. The reaction mixture was cooled, basified (5-M NaOH) filtered and the resulting solid suspended in MeOH, treated with HCl in dioxan (4-M, 2 mL), diluted with diethyl ether and filtered to give the title compound (419 mg, 94%) as a yellow solid.

WORKUP

后处理

  1. temperaturethen heated at 70° C. for 2 h
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. additiontreated with HCl in dioxan (4-M, 2 mL)
  5. additiondiluted with diethyl ether
  6. filtrationfiltered