反应详情

温度

60 °C

3-(2-[1,3]Dithietan-2-ylidene-2-pyridin-4-yl-acetyl)-benzonitrile (5 g, 16.1 mmol) was suspended in absolute ethanol (50 mL) and heated to 60° C. Hydrazine monohydrate (3.13 mL, 64.4 mmol, 4 eq) was added dropwise and the mixture was stirred at 60° C. for 2 hours. The suspension was concentrated to about ¼ of the original volume, diluted with THF (50 mL) and stirred for 5 minutes. The yellow solid was filtered, washed with THF and dried at 50° C. for 1 hours. The crude product (4.59 g) was used in the following step without further purification.

1. concentrationThe suspension was concentrated to about ¼ of the original volume
2. additiondiluted with THF (50 mL)
3. stirringstirred for 5 minutes
4. filtrationThe yellow solid was filtered
5. washwashed with THF
6. customdried at 50° C. for 1 hours
7. customThe crude product (4.59 g) was used in the following step without further purification