反应详情

温度

0 °C

To a solution of 6,7-dimethoxy-3-isoquinolinecarboxylic acid (6.99 g, 30.0 mmol) in 300 ml of N,N-dimethylformamide were added triethylamine (12.14 g, 120.0 mmol) and diphenyl chlorophosphate (80.6 g, 30.0 mmol) at 0° C. After stirring for 4 hours at 0° C., N-amino-2-oxoimidazolidine (3.03 g, 30.0 mmol) was added, and the mixture was stirred at 0° C. overnight. Ammonium salts (2.0 g) were filtered off, and the filtrate was evaporated in vacuo. The residue was triturated with a 1:1 mixture of water and ethyl acetate. The solid was filtered off and triturated twice with water at pH 8 for 3 hours. The remaining solid was filtered off, washed with water and dried in vacuo. Yield: 4.30 g; melting point 220° C. (dec.).

1. stirringthe mixture was stirred at 0° C. overnight
2. filtrationAmmonium salts (2.0 g) were filtered off
3. customthe filtrate was evaporated in vacuo
4. customThe residue was triturated with a 1:1 mixture of water and ethyl acetate
5. filtrationThe solid was filtered off
6. customtriturated twice with water at pH 8 for 3 hours
7. filtrationThe remaining solid was filtered off
8. washwashed with water
9. customdried in vacuo