反应详情

(R)-2-(Benzyl(2-(benzyloxy)ethyl)amino)-1-(3-nitrophenyl)ethanol (30.371 g) which can be prepared according to the method described in Reference example 57, etc. and imidazole (6.1318 g; manufactured by Tokyo Chemical Industry, Co., Ltd.) were dissolved in dehydrated DMF (150 mL), added with chlorotriethylsilane (15.1 mL; manufactured by Shin-Etsu Chemical Co., Ltd.), followed by stirring overnight at room temperature. The reaction solution was poured to water and extracted twice with ethyl acetate. The organic layer was washed twice with water and once with brine and dried over magnesium sulfate. After concentrating under reduced pressure, the residue was purified by column chromatography (“COLUMN-A”; n-hexane:ethyl acetate=100:0→87:13) to obtain the title compound (36.655 g).

1. extractionextracted twice with ethyl acetate
2. washThe organic layer was washed twice with water and once with brine
3. dry with materialdried over magnesium sulfate
4. concentrationAfter concentrating under reduced pressure
5. customthe residue was purified by column chromatography (“COLUMN-A”; n-hexane:ethyl acetate=100:0→87:13)