反应详情

温度

80 °C

A mixture of 1 g of N-methyl-2-nitrobenzenesulfonamide, 2.3 g of tert-butyl [(1R)-2-hydroxy-1-phenylethyl]carbamate, 2.5 g of triphenylphosphine, 4.2 ml of diethyl azodicarboxylate, and 40 ml of toluene was stirred at 80° C. for 2 hours, and the solvent was evaporated under reduced pressure. To a solution of the obtained residue in chloroform was added silica gel, followed by filtration, and the filtrate was concentrated under reduced pressure. To a solution of the obtained residue in 3 ml of dichloromethane was added 3 ml of trifluoroacetic acid, followed by stirring for 1 hour. The solvent was evaporated under reduced pressure, and an aqueous sodium carbonate solution and chloroform were then added thereto to carry out a layer separation operation. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 890 mg of N-[(2R)-2-amino-2-phenylethyl]-N-methyl-2-nitrobenzenesulfonamide.

1. customthe solvent was evaporated under reduced pressure
2. additionTo a solution of the obtained residue in chloroform was added silica gel
3. filtrationfollowed by filtration
4. concentrationthe filtrate was concentrated under reduced pressure
5. additionTo a solution of the obtained residue in 3 ml of dichloromethane was added 3 ml of trifluoroacetic acid
6. stirringby stirring for 1 hour
7. customThe solvent was evaporated under reduced pressure
8. additionan aqueous sodium carbonate solution and chloroform were then added
9. customa layer separation operation
10. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
11. customthe solvent was evaporated under reduced pressure
12. customThe obtained residue was purified by silica gel column chromatography