反应详情

Mix (3S,5R)-5-[(1S,2S)-1-benzyloxy-2-dibenzylamino-3-(3,5-difluorophenyl)-propyl]-3-methylmorpholin-2-ol (1.06 g, 1.85 mmol) with neopentanol (1.63 g, 18.5 mmol,) in dichloromethane (0.2 mL). Add 4 Å molecular sieves (850 mg), then methanesulphonic acid (2.4 mL, 37 mmol) and heat at 50° C. for 4 hours. Cool to room temperature, dilute with dichloromethane and add slowly to a solution of saturated aqueous sodium bicarbonate. Extract the aqueous layer with dichloromethane, dry (sodium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 100:0 to 90:10 hexanes:ethyl acetate) to give the desired compound as a white solid (665 mg, 56% yield).

1. additionAdd 4 Å molecular sieves (850 mg)
2. extractionExtract the aqueous layer with dichloromethane
3. dry with materialdry (sodium sulfate)
4. filtrationfilter
5. concentrationconcentrate
6. custompurify
7. wash(silica gel chromatography, eluting with 100:0 to 90:10 hexanes:ethyl acetate)