HRID2279616
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture is cooled to RT
- custompartitioned between EtOAc and water
- customseparate the layers
- extractionThe aqueous layer is extracted twice with further EtOAc
- customdried
- customevaporated
- customPurification by flash chromatography
- washeluting with a mixture of 7% MeOH and 1% TEA in DCM