反应详情

Triethylamine (10 ml, 71 mmol) and then, in portions, Pyr.SO3 (5.8 g, 36 mmol), were added at 0° C. to a solution of 4-(6-methoxy-quinazolin-4-yloxymethyl)-cyclohexanol (2.88 g, 10 mmol) in DMSO (30 ml). The reaction mixture was stirred at that temperature for 15 minutes and then allowed to come to room temperature. After 2 hours, water (300 ml) was added. The aqueous phase was extracted with ether (3×150 ml). The combined organic phases were washed with saturated sodium chloride solution, dried over MgSO4 and concentrated. The crude product was purified by chromatography on silica gel (EtOAc/hex 1/2).

1. customto come to room temperature
2. waitAfter 2 hours
3. extractionThe aqueous phase was extracted with ether (3×150 ml)
4. washThe combined organic phases were washed with saturated sodium chloride solution
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe crude product was purified by chromatography on silica gel (EtOAc/hex 1/2)