反应详情

A solution of methyl 2-chlorosulfonyl-6nitrobenzoate (2.80 g, 10 mmol) in 100 ml of THF was cooled to ice temperature and stirred in an ice-bath while a solution of 3-amino-1-propanol (99%) (1.67 g, 22 mmol) was added dropwise over a period of 45 minutes. Stirring in the ice-bath was continued for 30 minutes. The reaction mixture then was acidified by addition of 3.0 ml of 1.2 N HCl. The THF was evaporated under reduced pressure and the residue taken up in 100 ml of ethyl acetate. After extracting this solution with 4×20 ml of saturated NaCl solution, the ethyl acetate was evaporated and the residue recrystallized from a mixture of ethyl acetate and hexane to give 2.70 g (84.9%) of light yellow crystalline product, m.p., 87°-88.5°.

1. additionwas added dropwise over a period of 45 minutes
2. customThe THF was evaporated under reduced pressure
3. extractionAfter extracting this solution with 4×20 ml of saturated NaCl solution
4. customthe ethyl acetate was evaporated
5. customthe residue recrystallized from a mixture of ethyl acetate and hexane
6. customto give 2.70 g (84.9%) of light yellow crystalline product, m.p., 87°-88.5°