反应 #5339

反应方程式

methyl 2-butyl-1-[[2'-(acetoxycarbamimidoyl)biphenyl-4yl)methyl]benzimidazole-7-carboxylate

CS2

sodium hydride

→

prisms

收率 32.0%

Methyl 2-butyl-1-[[2'-(2,5-dihydro-5-thioxo-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl]benzimidazol-7-carboxylate

收率 32.0%

溶剂

DMF

反应条件

后处理

1. 1
   萃取The mixture was extracted with ethylacetate
2. 2
   洗涤the extract was washed with water
3. 3
   其他dried
4. 4
   浓缩concentrated to dryness
5. 5
   其他The residue was crystallized from chloroformmethanol

实验过程

To a mixture of methyl 2-butyl-1-[[2'-(acetoxycarbamimidoyl)biphenyl-4yl)methyl]benzimidazole-7-carboxylate (2.0 g) and CS2 (1.5 g) in DMF (12 ml) gas added sodium hydride (60% in oil, 0.56 g) during a period of 10 minutes and the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into ice-water and the pH of the solution was adjusted to 3. The mixture was extracted with ethylacetate and the extract was washed with water, dried, and concentrated to dryness. The residue was crystallized from chloroformmethanol to afford pale yellow prisms (0.64 g, 32 %). m.p. 180°-181° C.

来源