反应详情

A solution of 4-benzyl-2-methyl-5-oxo-morpholine-3-carboxylic acid ethyl ester (0.24 g, 0.865 mmol; prepared according to the procedure described in Meinzer A. et al., Helv. Chim. Acta 2004, 87, 90-105) in tetrahydrofuran (7 ml) was cooled to −20° C. and borane-methyl sulfide complex (0.246 ml, 2.595 mmol) was added dropwise. The resulting mixture was allowed to warm to room temperature and stirred overnight. After the addition of methanol (5 ml), stirring was continued for 1 h. The solution was diluted with dichloromethane, washed with brine, and concentrated in vacuo. The resulting 4-benzyl-2-methyl-morpholine-3-carboxylic acid ethyl ester was used in the next step without further purification. LC/MS (method 8): Rt=0.54 min; m/z=264.25 (M+H+).

1. customprepared
2. additionborane-methyl sulfide complex (0.246 ml, 2.595 mmol) was added dropwise
3. stirringstirring
4. waitwas continued for 1 h
5. washwashed with brine
6. concentrationconcentrated in vacuo
7. customThe resulting 4-benzyl-2-methyl-morpholine-3-carboxylic acid ethyl ester was used in the next step without further purification