反应详情

温度

20 °C

A four neck flask (3 liters) equipped with a thermometer and a stirrer was charged with 573.2 g (6.0 mole) of guanidine hydrochloride and 1.5 liter of methanol and cooled to 20° C. Slowly dropwise added thereto was 324.1 g (6.0 mole) of sodium methoxide crystal at 20° C. or lower and stirred for 3 hours. Deposited crystals were filtered off. The mother liquor was charged to the four neck flask (3 liters) equipped with the above devices, and 337.4 g (2.4 mole) of benzoyl chloride was slowly dropwise added at 15° C. or lower and stirred for 12 hours. Deposited crystals were filtered off, and the mother liquor was concentrated under reduced pressure to obtain white crystals. The resulting crystals were sufficiently washed with 3 liters of deionized water and dried under reduced pressure, whereby the intended compound (white crystals) was obtained.

1. customA four neck flask (3 liters) equipped with a thermometer and a stirrer
2. additionSlowly dropwise added
3. customat 20° C.
4. filtrationDeposited crystals were filtered off
5. additionThe mother liquor was charged to the four neck flask (3 liters)
6. additionwas slowly dropwise added at 15° C.
7. stirringlower and stirred for 12 hours
8. filtrationDeposited crystals were filtered off
9. concentrationthe mother liquor was concentrated under reduced pressure
10. customto obtain white crystals
11. washThe resulting crystals were sufficiently washed with 3 liters of deionized water
12. customdried under reduced pressure, whereby the intended compound (white crystals)
13. customwas obtained