反应详情

The slurry of Description 9 was cooled to 50±3° and isopropanol (30 ml) added, followed by an aqueous solution of benzene sulfonic acid (32% w/v, 10 ml). The mixture was cooled to 22±3° over ca 1 h, seeded with authentic 4-({[({[(2S)-4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}amino)carbonyl]amino}methyl) benzamide hydrate and aged at 22±3° for 72 h. The mixture was cooled to 0±3° over 1 h and filtered. The filter cake was washed with a 4:1:0.1 mixture of isopropyl acetate/isopropyl alcohol/water (2.5 ml) and dried in vacuo at 25±5° to give the title compound as a white solid (6.9 g).

1. temperatureThe slurry of Description 9 was cooled to 50±3°
2. temperatureThe mixture was cooled to 22±3° over ca 1 h
3. temperatureThe mixture was cooled to 0±3° over 1 h
4. filtrationfiltered
5. washThe filter cake was washed with a 4:1:0.1 mixture of isopropyl acetate/isopropyl alcohol/water (2.5 ml)
6. customdried in vacuo at 25±5°