反应详情

To a 0° C. solution of 1-benzhydryl-3-methylazetidin-3-ol (70 g, 276 mmol) and TEA (53.1 g, 525 mmol) in DCM (700 mL) was added drop-wise methanesulfonyl chloride (57 g, 497 mmol). The reaction mixture was stirred for 2 h then filtered and the filter cake was washed with DCM (3×50 mL). The filtrate was washed with water (3×100 mL), dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated in vacuo to give methanesulfonic acid 1-benzhydryl-3-methyl-azetidin-3-yl ester (90 g, 98%) as a brown solid, which was used in the next step without further purification. 1H NMR (CDCl3, 400 MHz): δ 7.44 (m, 4H), 7.33 (m, 4H), 7.26 (m, 2H), 4.55 (brs, 1H), 3.46 (m, 4H), 3.07 (s, 3H), 1.94 (s, 3H).

1. filtrationthen filtered
2. washthe filter cake was washed with DCM (3×50 mL)
3. washThe filtrate was washed with water (3×100 mL)
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationThe filtrate was concentrated in vacuo