HRID970461
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
PROCEDURE
实验过程
To a solution of 4-piperazinopyrido[3′,2′;4,5]thieno[3,2-d] pyrimidine (200 mg, 0.74 mmol) and pyridine (0.5 mL, 7.9 mmol) in dichloromethane (20 mL) was added a solution of product 1d in dichloromethane (20 mL) and this was stirred overnight. Methanol was added to quench excess thiophosgene, and the residue after removal of solvent was purified by silica gel column chromatography eluting with 5% methanol/dichloromethane and further recrystallized from dichloromethane/hexane to give 60 mg (15%).
WORKUP
后处理
- customto quench excess thiophosgene
- customthe residue after removal of solvent
- customwas purified by silica gel column chromatography
- washeluting with 5% methanol/dichloromethane
- customfurther recrystallized from dichloromethane/hexane
- customto give 60 mg (15%)