Hydrochloric Acid → 4687-08-5
反応式
C[C@H]([O:10][C:11](=[O:31])[C@@H:12]([C:24]1[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=1)[O:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=1)C(=O)N1CCCC1.O.Cl>C1(C)C=CC=CC=1>[Cl:30][C:27]1[CH:26]=[CH:25][C:24]([CH:12]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:21])([F:22])[F:23])[CH:15]=2)[C:11]([OH:31])=[O:10])=[CH:29][CH:28]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
To the residue prepared in STEP C above was added water (10 g) and a 36-38% HCl solution (60 g). The resulting biphasic mixture was stirred at 80° C. for between about 4 and about 8 hours (till completion of the hydrolysis as determined by HPLC) The resulting mixture was then cooled to 60° C. and toluene (125 mL) added. The aqueous phase was discarded and the organic phase washed with water (50 mL). Toluene (about 80 g) was removed by distillation to dry the organic phase. The resulting solution was then cooled to 70° C. and petrol ether 60/90 (250 mL) was added. The resulting solution was further cooled to 37° C. and seeded. The resulting mixture was stirred for 30 minutes at 37° C., the resulting suspension then cooled to 0° C. over about 2.5 hours. The precipitated crystals were filtered off and washed with a mixture of toluene (5 mL 0 and petrol ether 60/90 (9 mL) to yield wet product. The wet product was dried in a vacuum at 30° C. to yield the title compound as an off-white solid.