HRID2046232

反应详情

EQUATION

反应方程式

HRID 2046232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 1M solution of lithium aluminum hydride was added to a stirred solution of 3-chloro-4-oxo-4,5,6,7-tetrahydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid ethyl ester (0.37 g, 1.51 mmol) in THF (15 mL) at 0° C. The mixture was stirred at room temperature for 2 hours and then diluted with AcOEt. Na2SO4.10H2O was added at 0° C. and the mixture stirred for 15 minutes at 0° C., filtered through a pad of diatomaceous earth and then washed with additional THF. The solvents were evaporated in vacuo to yield 3-chloro-2-hydroxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (0.24 g, 79% yield) that was used in the next step without further purification.

WORKUP

后处理

  1. stirringthe mixture stirred for 15 minutes at 0° C.
  2. filtrationfiltered through a pad of diatomaceous earth
  3. washwashed with additional THF
  4. customThe solvents were evaporated in vacuo