HRID2178895

反应详情

EQUATION

反应方程式

HRID 2178895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a suspension of lithium aluminum hydride (0.32 g, 8.4 mmol) in THF (15 mL) was added a solution of tert-butyl 4-(4-nitro-1H-pyrazol-1-yl)piperidine-1-carboxylate (500 mg, 1.7 mmol) in THF (10 mL) and the reaction mixture was stirred with heat at 60° C. for 16 h. The reaction mixture was cooled to 0° C. and quenched by the slow addition of ethanol (0.3 mL) then water (0.3 mL) and finally 3 N NaOH aq. (0.3 mL). The resulting mixture was stirred for 30 min, filtered and the filtrate was concentrated and dried to obtain the desired product (280 mg) which was used without any purification: ESI MS m/z 181 [M+H]+.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customquenched by the slow addition of ethanol (0.3 mL)
  3. stirringThe resulting mixture was stirred for 30 min
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated
  6. customdried