反应详情

23.7 g 4-Hydroxy-3,3-dimethyl-butan-2-one was dissolved in 150 mL DCM. 49.5 mL (3 eq) pyridine and 17.5 mL (1.1 eq) mesylchloride were added and the mixture was stirred at room temperature for 20 hours. The suspension was filtered and the filter cake was washed two times with DCM. The filtrate was washed with 1 M HCl and the aqueous layer was extracted two times with DCM. The combined filtrates were dried over Na2SO4 and the solvent was evaporated under reduced pressure to give 41.2 g of a brown liquid. 1H NMR (400 MHz, CDCl3) δ 1.24 (s, 6H), 2.20 (s, 3H), 3.03 (s, 3H), 4.21 (s, 2H).

1. filtrationThe suspension was filtered
2. washthe filter cake was washed two times with DCM
3. washThe filtrate was washed with 1 M HCl
4. extractionthe aqueous layer was extracted two times with DCM
5. dry with materialThe combined filtrates were dried over Na2SO4
6. customthe solvent was evaporated under reduced pressure