反应详情

To a solution ethyl 2,6-difluoro-4-[(3-hydroxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalene-2-carbonyl)-amino]-benzoate (Compound C, 227 mg, 0.52 mmol) in 10 ml of anhydrous dichloromethane under nitrogen at 25° C. was added sulfuryl chloride (0.0413 ml, 0.57 mmol) and anhydrous ethyl ether (0.054 ml, 0.52 mmol). Reaction was instantaneous at 25° C. as monitored by 1H NMR. The reaction mixture was quenched with saturated NaHCO3 then extracted with ethyl acetate. The organic layer was washed with water, brine and dried over Na2SO4. The title compound was obtained as a white solid after column chromatography with ethyl acetate:hexane (1:9).

1. customReaction
2. customwas instantaneous at 25° C.
3. customThe reaction mixture was quenched with saturated NaHCO3
4. extractionthen extracted with ethyl acetate
5. washThe organic layer was washed with water, brine
6. dry with materialdried over Na2SO4