反应详情

温度

0 °C

8.24 g (47.0 mmol) (2-Hydroxy-propyl)-carbamic acid tert-butyl ester were dissolved in 100 ml dichloromethane. 7.8 ml (1.2 equiv.) triethylamine were added and the mixture was cooled to 0° C. At that temperature 4.37 ml (1.2 equiv.) methanesulfonyl chloride were added dropwise. The resulting solution was allowed to reach room temperature and stirred for further 4 h. The mixture was diluted with 100 ml dichloromethane and washed sequentially with a 5% KHSO4-solution, water and brine. The organic phase was dried over anhydrous MgSO4 and concentrated under reduced pressure to give methanesulfonic acid 2-tert-butoxycarbonylamino-1-methyl-ethyl ester in crude form as yellow oil.

1. customto reach room temperature
2. washwashed sequentially with a 5% KHSO4-solution, water and brine
3. dry with materialThe organic phase was dried over anhydrous MgSO4
4. concentrationconcentrated under reduced pressure