反应详情

温度

68 °C

The concentrate obtained in Working Example 2(2) (methyl2-[N-t-butoxycarbonyl-N-[(2′-cyanobiphenyl-4-yl)methyl]amino]-3-nitro-benzoate [BBN]) and methanol (3200 L) were mixed, and 35% concentrated hydrochloric acid (1050 L) was added to the mixture at 30° C. or less for about 4 hours. The mixture was heated to reflux temperature (67-69° C.) at a speed of 10° C. or less/hour, and stirred for about 1.5 hours under reflux. The reaction solution was cooled, to which was added methanol (800 L), and the solution was stirred at 3-10° C. for about 1 hour. The precipitated crystals were separated, washed with methanol and dried to give methyl 2-[[(2′-cyano-biphenyl-4-yl)methyl]amino]-3-nitro-benzoate [MBN] (407 kg; yield based on MPB: 75%).

1. additionwere mixed
2. temperatureThe mixture was heated
3. temperatureunder reflux
4. temperatureThe reaction solution was cooled, to which
5. stirringthe solution was stirred at 3-10° C. for about 1 hour
6. customThe precipitated crystals were separated
7. washwashed with methanol
8. customdried