HRID1080442
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A stirred solution of 6-methoxy-3-(1-piperazinyl)-1,2-benzisoxazole (1.0 g), 4,6-dichloropyrimidine (0.64 g) and sodium bicarbonate (1.08 g) were refluxed in absolute ethanol under N2 for 90 minutes. TLC (silica gel 2/1 acetone/heptane) showed no presence of starting material. The reaction was allowed to cool to room temperature, partitioned between CH2Cl2 and water, extracted with CH2Cl2, dried over MgSO4 and concentrated in vacuo to afford 1.44 g of material. The material was further purified through recrystallization from CH2Cl2 /pet. ether to yield the product 1.1 g, m.p. 203°-204° C.
WORKUP
后处理
- custompartitioned between CH2Cl2 and water
- extractionextracted with CH2Cl2
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo