反应详情

To a solution of (R)-3-(4-(2-(4-((S)-3-chloro-2-hydroxypropoxy)phenyl)propan-2-yl)phenoxy)propane-1,2-diol (1000 mg, 2.53 mmol) in anhydrous dichloromethane (8.0 mL) at −78° C. were successively added 2,6-lutidine (590 μL, 5.06 mmol) and acetic chloride (144 μL, 2.02 mmol) dropwise. After 1 h, the reaction mixture was quenched with an aqueous solution of sodium chloride and stirred for 15 min, and the resulting mixture was extracted twice with dichloromethane. The organic phases were combined, dried over anhydrous magnesium sulfate and filtered. Solvents were evaporated, and the resulting crude material was purified by silica gel flash chromatography (eluent: 2% methanol in dichloromethane) to provide the title compound (300 mg, 27%) as a sticky solid.

1. customat −78° C.
2. customthe reaction mixture was quenched with an aqueous solution of sodium chloride
3. extractionthe resulting mixture was extracted twice with dichloromethane
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customSolvents were evaporated
7. customthe resulting crude material was purified by silica gel flash chromatography (eluent: 2% methanol in dichloromethane)