HRID536028

反应详情

EQUATION

反应方程式

HRID 536028 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

A mixture of 2-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (4.0 g, 9.16 mmol), NaCN (0.67 g, 13.74 mmol), NaI (2.0 g, 9.16 mmol) and DMF (30 ml) were stirred for 48 hrs at 60° C. Reaction mixture was cooled to 20-25° C. and water was added and solid filtered off. The crude product was purified by column chromatography using silica gel (100-200 mesh) and 2 to 4% methanol in DCM as an eluent to obtain 6-Oxo-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-6,7-dihydro-1H-purine-2-carbonitrile (2.6 g, 67%) as an off white solid.

WORKUP

后处理

  1. customReaction mixture
  2. temperaturewas cooled to 20-25° C.
  3. filtrationsolid filtered off
  4. customThe crude product was purified by column chromatography