反应详情

温度

2 °C

Methanesulfonyl chloride (1.73 ml, 22.5 mmol) was added to a cooled (ice bath, 0-4° C.), stirred solution of (R)-3-hydroxy-piperidine-carboxylic acid tert-butyl ester (3.0 g, 15 mmol) and triethylamine (3.12 ml, 22.5 mmol) in dichloromethane (30 ml). Following the addition the reaction was stirred at this temperature for 30 minutes before being allowed to warm to ambient temperature. After stirring at ambient temperature for 2 hours, aqueous sodium hydrogen carbonate (50 ml) was added, followed by vigorous stirring for 30 minutes. The reaction was diluted with dichloromethane (300 ml) and aqueous sodium hydrogen carbonate (300 ml) and after partitioning the organic phase was washed with water (200 ml), dried with magnesium sulphate and evaporated to dryness under reduced pressure to yield (R)-3-methanesulfonyloxypiperidine-1-carboxylic acid tert-butyl ester as a semi-crystalline solid.

1. additionthe addition the reaction
2. temperatureto warm to ambient temperature
3. stirringAfter stirring at ambient temperature for 2 hours
4. stirringby vigorous stirring for 30 minutes
5. customafter partitioning the organic phase
6. washwas washed with water (200 ml)
7. dry with materialdried with magnesium sulphate
8. customevaporated to dryness under reduced pressure