反应详情

温度

110 °C

Sodium hydrosulfite (86%, 233 g) was suspended in dimethylformamide (240 ml) and the suspension was heated to 110° C. To this suspension was added dropwise at 110° C. a solution of 2-(5-fluoro-2-nitroanilino)benzo[b]thiophene-3-carbonitrile (120 g), dimethylformamide (720 ml) and water (27.5 ml), which solution had been heated to 65-70° C. The reaction mixture was stirred at 110° C. for 1 hour and cooled to 20° C. Water (3.3 L) was added in 6 portions over 1 hour and the mixture was stirred at 20° C. for 1.5 hours. The precipitated crystals were filtered by suction and washed with water (2 L) to give 2-(2-amino-5-fluoroanilino)benzo[b]thiophene-3-carbonitrile (158 g, (wet weight)) as ocher crystals.

1. temperaturehad been heated to 65-70° C
2. temperaturecooled to 20° C
3. stirringthe mixture was stirred at 20° C. for 1.5 hours
4. filtrationThe precipitated crystals were filtered by suction
5. washwashed with water (2 L)