HRID257424

反应详情

EQUATION

反应方程式

HRID 257424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customfollowed by reaction at 80°-90° C. for about 40 hours
  2. customDMF was removed by distillation
  3. customthe residue was purified by silica gel column chromatography (eluent: chloroform: methanol=13:1 (v/v))
  4. customRecrystallization from methanol-ether