反应详情

To a nitrogen purged flask fitted with an overhead stirrer, a thermometer, and a condenser is added 20 kg (37.8 mol) of 1-(3,3-diethoxypropyl)-5-(4-fluorophenyl)-2-(1-methylethyl)-N,4-diphenyl- 1 H-pyrrole-3-carboxamide along with 200 L of acetone. The solution is stirred and 100 L of 2N hydrochloric acid solution is added. The mixture is heated to reflux for four hours then cooled to 50° C.±5° C., seeded, and cooled to 0° C.±5° C. The produce is collected by filtration, washed with 100 L 2-propanol-water (1:1) and dried in vacuo at 50° C. for 64 hours to yield 16.2 kg of 5-(4-fluorophenyl)-2-(1-methylethyl)-1-(3-oxopropyl)-N,4-diphenyl-1 H-pyrrole-3-carboxamide as an off-white solid.

1. customTo a nitrogen purged flask fitted with an overhead stirrer
2. temperatureThe mixture is heated
3. temperatureto reflux for four hours
4. temperaturethen cooled to 50° C.±5° C.
5. temperaturecooled to 0° C.±5° C
6. filtrationThe produce is collected by filtration
7. washwashed with 100 L 2-propanol-water (1:1)
8. customdried in vacuo at 50° C. for 64 hours