反应详情

温度

2.5 °C

A solution of methanesulfonyl chloride (28 ml, 0.36 mole) in dichloromethane (50 ml) was added dropwise to a solution of piperidine-4-carboxylic acid ethyl ester (50 grams, 0.32 mole) and triethylamine (53 ml, 0.38 mole) in dichloromethane (350 ml) at 0° C. The reaction mixture was stirred at 0-5° C. for 3 hours. The solution was washed with 2×100 ml water, dried (anhydrous magnesium sulfate) and concentrated under reduced pressure. The solid residue was triturated with 100 ml ethyl ether, collected by filtration and dried to give 1-methanesulfonylpiperidine-4-carboxylic acid ethyl ester (68 grams, 90%), m.p. 91-92° C.

1. washThe solution was washed with 2×100 ml water
2. dry with materialdried (anhydrous magnesium sulfate)
3. concentrationconcentrated under reduced pressure
4. customThe solid residue was triturated with 100 ml ethyl ether
5. filtrationcollected by filtration
6. customdried