反应详情

A solution of methyl 2-chlorosulfonyl-6-nitrobenzoate (2.80g, 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%) (1.67g, 22 mmol) was added dropwise over a period of 45 minutes. Stirring in the ice-bath was continued for 30 minutes. The reaction miture than was acidified by addition of 3.0 ml of 1.2N 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 2.70g (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 2.70g (84.9%) of light yellow crystalline product, m.p., 87-88.5°