反应详情

温度

95 °C

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.

1. temperatureThe mixture was cooled to room temperature
2. filtrationThe precipitated product was filtered
3. washwashed with water
4. customto yield
5. customafter drying
6. custom62.8 g of the title compound as yellow crystals (purity: 86.4% by HPLC) which could be further purified by recrystallization