反应详情

温度

0 °C

To a solution of 3,4-diflorobenzoyl chloride (45 mL, 358 mmol) in acetonitrile (1.43 L) was added solid potassium thiocyanate (KNCS) (38.2 g, 393 mmol). The suspension was stirred to 0° C. for 10 min and then the cooling bath was removed. The suspension was stirred at room temperature for an additional 20 min. A solution of 2-chloro-4-fluorobenzylamine (57.1 g, 358 mmol) in acetonitrile (150 mL) was added over 5 minutes. The resulting suspension was stirred at room temperature for 3 hours. The reaction mixture was diluted with water (1.4 L) and stirred for 1 hour. The suspension was filtered, rinsed with water (150 mL) and dried in vacuo at 60° C. to afford N-((2-chloro-4-fluorobenzyl)carbamothioyl)-3,4-difluorobenzamide as a yellow solid (98.3 g, 77% yield). 1HNMR (400 MHz, DMSO-d6) δ 11.56 (bs, 1H), 11.12 (t, 1H, J=5.7 Hz), 8.00 (m, 1H), 7.79 (m, 1H), 7.54 (m, 1H), 7.44 (m, 2H), 7.19 (m, 1H), 4.85 (d, 2H, J=5.7 Hz).

1. customthe cooling bath was removed
2. stirringThe suspension was stirred at room temperature for an additional 20 min
3. stirringThe resulting suspension was stirred at room temperature for 3 hours
4. stirringstirred for 1 hour
5. filtrationThe suspension was filtered
6. washrinsed with water (150 mL)
7. customdried in vacuo at 60° C.