反应详情

To a solution of (1,4-dioxa-spiro[4.5]dec-8-yl)-methanol (1.0 g, 5.8 mmol, 1.0 eq.) and ethyldiisopropylamine (17 mL, 3.0 eq.) in methylene chloride (4 mL) at 0° C. was added dropwise MsCl (0.46 mL, 1.0 eq.) and the resulting mixture was warmed to room temperature and stirred for 2 h. The reaction was quenched by addition of sat. NaHCO3 and the separated aqueous phase was extracted with 3× methylene chloride and 4×EtOAc. The combined organic phase was dried over Na2SO4, filtered and concentrated to give a crude methanesulfonic acid 1,4-dioxa-spiro[4.5]dec-8-ylmethyl ester.

1. customThe reaction was quenched by addition of sat. NaHCO3
2. extractionthe separated aqueous phase was extracted with 3× methylene chloride and 4×EtOAc
3. dry with materialThe combined organic phase was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated