تفاعل #5338

معادلة التفاعل

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

المردود 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

المردود 57.6%

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction mixture was partitioned between ethyl acetate (50 ml) and 1N HCl (20 ml)
2. 2
   غسيلThe organic layer was washed with water
3. 3
   أخرىdried
4. 4
   تركيزconcentrated to dryness
5. 5
   أخرىThe residue was crystallized from chloroformethyl acetate

الإجراء التجريبي

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).

المصدر