反应 #5338

反应方程式

crude crystals

Methyl 2-ethoxy-1-[[2'-(ethoxycarbonyloxy-carbamimidoyl)biphenyl-4-yl]methyl]benzimidazole-7-carboxylate

1,8-diazabicyclo[5.4.0]undec-7-ene

→

title compound

收率 57.6%

Methyl 2-ethoxy-1-[[2'-(2,5-dihydro-5-oxo-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl]benzimidazole-7-carboxylate

收率 57.6%

溶剂

ethyl acetate

反应条件

后处理

1. 1
   其他The reaction mixture was partitioned between ethyl acetate (50 ml) and 1N HCl (20 ml)
2. 2
   洗涤The organic layer 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 chloroformethyl acetate

实验过程

The crude crystals (4.0 g) obtained in Example (57b) was dissolved in ethyl acetate (50 ml). To the solution was added 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU, 3.2 g), and the mixture was stirred for 2 hours at 80° C. The reaction mixture was partitioned between ethyl acetate (50 ml) and 1N HCl (20 ml). The organic layer was washed with water, dried and concentrated to dryness. The residue was crystallized from chloroformethyl acetate to afford the title compound as colorless prisms (2.1 g, 45%), which was in agreement with that obtained in Example (1d).

来源