Sodium Hydroxide → N-(5-amino-2-chloro4-fluorophenyl)-1-chloromethanesulfonamide
反応式
[Cl:1][C:2]1[C:7]([NH:8][S:9]([CH2:12][Cl:13])(=[O:11])=[O:10])=[CH:6][C:5]([NH:14]C(=O)C)=[C:4]([F:18])[CH:3]=1.[OH-].[Na+]>Cl>[NH2:14][C:5]1[C:4]([F:18])=[CH:3][C:2]([Cl:1])=[C:7]([NH:8][S:9]([CH2:12][Cl:13])(=[O:11])=[O:10])[CH:6]=1参加物
4
反応条件
- 温度
- 95 °C
実験手順
74.5 g of crude N-[4-chloro-5-[[(chloromethyl)sulfonyl]amino]-2-fluorophenyl]acetamide (purity: 90%) was suspended in 355 mL of 6 N hydrochloric acid and heated to 95° C. After 1.5 hours the suspension turned into a solution. The mixture was cooled to room temperature and 90 mL of a NaOH solution (50%) was added (pH 3). The precipitated product was filtered and washed with water to yield, after drying, 62.8 g of the title compound as yellow crystals (purity: 86.4% by HPLC) which could be further purified by recrystallization as described above in Example 5.