反应详情

温度

0 °C

Add trimethyloxonium tetrafluoroborate (530.7 g) to a solution of 2-oxopiperidine-4-carboxylic acid ethyl ester (307.7 g, 1.80 mol) in dry dichloromethane (4.68 L) under nitrogen, and stir the reaction at room temperature for 16 hours. Cool the mixture to 0° C. and adjust to pH 8 with saturated aqueous sodium bicarbonate. Separate the layers and extract the aqueous phase with additional dichloromethane (2×1 L). Combine the organic phases, dry over magnesium sulfate, filter, and concentrate to provide the title compound (273.68 g). Mass spectrum (m/z): 186 (M+1).

1. customthe reaction at room temperature for 16 hours
2. customSeparate the layers
3. extractionextract the aqueous phase with additional dichloromethane (2×1 L)
4. dry with materialCombine the organic phases, dry over magnesium sulfate
5. filtrationfilter
6. concentrationconcentrate