反应详情

To a solution of methyl 2-(3-amino-1-methylpiperidin-3-yl)acetate (186 mg, 1 mmol) and Et3N (0.42 mL, 3 mmol) in CH2Cl2 was added the solution of 2-chloroethyl chlorosulfonylcarbamate in CH2Cl2 (0.77 M, 1.3 mL, 1 mmol). After addition, the resulting mixture was stirred overnight at rt. Evaporation of solvents gave a light yellow oil which was used without further purification. A solution of this crude mixture, N-methyl-4-octylaniline (241 mg, 1.1 mmol) and Et3N (0.42 mL, 3 mmol) in CH3CN (10 mL) was refluxed for 2 h. After cooling to rt and evaporating solvents, the residue was purified by a short column (EtOAc/hexance=10:1) to give the title compound (105 mg, 22%) as white solid. MS ESI 468.3 [M+H]+, calcd for [C24H41N3O4S+H]+ 468.29.

1. additionAfter addition
2. customEvaporation of solvents
3. customgave a light yellow oil which
4. customwas used without further purification
5. temperatureAfter cooling to rt
6. customevaporating solvents
7. customthe residue was purified by a short column (EtOAc/hexance=10:1)