反应详情

To a solution of KOH (16.5 g, 294 mmol) in H2O (75 ml) was added 4-(methylamino)butyric acid hydrochloride (10, 15.1 g, 98.1 mmol) and the reaction mixture was cooled with an icebath. A solution of 3-(trifluoromethyl)benzene-sulfonyl chloride (9, 12.0 g, 49.1 mmol) in THF (75 ml) was dropwise added to the reaction mixture and stirring was continued at room temperature overnight. Aqueous 6 M HCl (75 ml) was added to the reaction mixture while cooling with an icebath, after which CH2Cl2 was added. The organic layer was separated, washed with brine, dried (Na2SO4), concentrated and co-evaporated with a minimal amount of Et2O. Crystallization of the residue out of EtOAc/heptane resulted in S-13 (11.32 g, 71%).

1. temperaturethe reaction mixture was cooled with an icebath
2. temperaturewhile cooling with an icebath
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated and co-evaporated with a minimal amount of Et2O
7. customCrystallization of the residue out of EtOAc/heptane
8. customresulted in S-13 (11.32 g, 71%)