HRID257424
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
The carboxyamide compound (0.37 g, 27 mmol) obtained in (a) described above and 1,2,2-trimethylpropyl isothiocyanate (1.15 g, 8.03 mmol) were added to 2 ml of DMF, followed by reaction at 80°-90° C. for about 40 hours. DMF was removed by distillation, and the residue was purified by silica gel column chromatography (eluent: chloroform: methanol=13:1 (v/v)). Recrystallization from methanol-ether gave 0.4 g of the intended product (yield: 53%).
WORKUP
后处理
- customfollowed by reaction at 80°-90° C. for about 40 hours
- customDMF was removed by distillation
- customthe residue was purified by silica gel column chromatography (eluent: chloroform: methanol=13:1 (v/v))
- customRecrystallization from methanol-ether