反应详情

温度

85 °C

To a stirred suspension of 7 g of 5-fluoroisatin in 58 ml of water was added a solution of 9.36 g of sodium hydroxide in 33 ml of water. The solution was heated to 85° C. and a solution of 12 g of 2-amino-1-(4-chlorophenyl)ethanone hydrochloride in a mixture of 92 ml of ethanol and 40 ml of tetrahydrofuran and 92 ml of water was added drop-wise over 2 hours. After the addition was complete, the solution was refluxed for an additional 30 minutes and then the ethanol and tetrahydrofuran were removed by distillation. The mixture was cooled to 20° C. and filtered through celite. The filtrate was acidified to pH 4 with acetic acid. The solid was filtered off, washed with water and dried, giving 12.8 g of the desired compound as a yellow solid, mp 241°-243° C.

1. additionwas added drop-wise over 2 hours
2. additionAfter the addition
3. temperaturethe solution was refluxed for an additional 30 minutes
4. customthe ethanol and tetrahydrofuran were removed by distillation
5. temperatureThe mixture was cooled to 20° C.
6. filtrationfiltered through celite
7. filtrationThe solid was filtered off
8. washwashed with water
9. customdried