HRID2279616

反应详情

EQUATION

反应方程式

HRID 2279616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
165 °C

PROCEDURE

实验过程

A mixture of 3-methyl-1H-pyrazole-4-carboxylic acid (adamantan-1-ylmethyl)-amide (1.6 g, 5.85 mmol), 4-amino-2-chloro-5-methylpyrimidine (924 mg, 6.4 mmol) and potassium carbonate (1.6 g, 11.7 mmol) in DMSO (10 mL) is heated at 165° C. for 14 h. The mixture is cooled to RT and partitioned between EtOAc and water and separate the layers. The aqueous layer is extracted twice with further EtOAc. The extracts are combined, dried and evaporated. Purification by flash chromatography eluting with a mixture of 7% MeOH and 1% TEA in DCM affords the title compound.

WORKUP

后处理

  1. temperatureThe mixture is cooled to RT
  2. custompartitioned between EtOAc and water
  3. customseparate the layers
  4. extractionThe aqueous layer is extracted twice with further EtOAc
  5. customdried
  6. customevaporated
  7. customPurification by flash chromatography
  8. washeluting with a mixture of 7% MeOH and 1% TEA in DCM