反应详情

A solution of methyl 2-chlorosulfonyl-6-nitrobenzoate (2.80 g, 10 mmol) in 100 ml of THF was cooled in an ice-bath and stirred while a solution of 1-amino-2-propanol (1.65 g, 22 mmol) in 10 ml of THF was added dropwise over a period of 50 minutes. After stirring an additional 30 minutes in the ice-bath, the reaction mixture was acidified by the addition of 3 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 with 4×20 ml of saturated NaCl solution, the ethyl acetate solution was dried over Na2SO4 and the solvent evaporated. The residue was crystallized from a mixture of ethyl acetate and hexane to give 2.02 g (63.5%) of yellow crystalline product, m.p., 93.5°-95°.

1. additionwas added dropwise over a period of 50 minutes
2. customThe THF was evaporated under reduced pressure
3. extractionAfter extracting with 4×20 ml of saturated NaCl solution
4. dry with materialthe ethyl acetate solution was dried over Na2SO4
5. customthe solvent evaporated
6. customThe residue was crystallized from a mixture of ethyl acetate and hexane