反应详情

温度

0 °C

To a stirred solution of (4-bromomethyl-2-methyl-benzyloxy)-tert-butyl-diphenyl-silane (3 g, 6.83 mmol) in tetrahydrofuran is added sec-butyl lithium at −78° C. under nitrogen atmosphere. The reaction mixture is warmed to 0° C. and stirred for 30 min. The reaction mixture is cooled to −78° C., N-formyl piperidine (1.13 mL, 10.24 mmol) is added, and the reaction mixture is stirred for 3 hours at room temperature. The reaction mixture is quenched with water at 0° C. and extracted with EtOAc (50 mL×3). The combined organic layer is washed with brine solution, dried over magnesium sulphate, and concentrated under vacuum to give the title compound (3 g, 46%). ESI/MS m/z 389.1 (M+H)+.

1. temperatureThe reaction mixture is cooled to −78° C.
2. stirringthe reaction mixture is stirred for 3 hours at room temperature
3. customThe reaction mixture is quenched with water at 0° C.
4. extractionextracted with EtOAc (50 mL×3)
5. washThe combined organic layer is washed with brine solution
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated under vacuum