反应详情

A solution of 4 g (0.02 mol) of 2-(1-methyl-3-pyrrolidinyl)-1H-benzimidazole in 100 mL of CH2Cl2 was added dropwise to a solution of 12.5 (0.025 mol) of 20% phosgene/toluene in 30 mL of CH2Cl2. The solution was stirred for 2 h, and 10 g (0.1 mol) of triethylamine was added dropwise. Stirring was continued for 2 h and the solution was extracted with dilute NaOH. The organic layer was dried (Na2SO4) and concentrated. The residue was crystallized twice from isopropyl ether. Yield 1.5 g (28%), mp 88°-91° C.

1. stirringStirring
2. waitwas continued for 2 h
3. extractionthe solution was extracted with dilute NaOH
4. dry with materialThe organic layer was dried (Na2SO4)
5. concentrationconcentrated
6. customThe residue was crystallized twice from isopropyl ether