反应详情

温度

120 °C

A mixture of 2-[4-(3-chloropropoxy)phenyl]-4,4-dimethyl-4,5-dihydro-1,3-oxazole ax10 (0.25 g, 0.9 mmol, 1 eq), 0.15 g of (2R)-2-methylpyrrolidine hydrochloride (1.2 mmol, 1.4 eq) and triethylamine (0.3 ml, 2.2 mmol, 2.4 eq) is stirred under microwave irradiation (120° C., 3.75 h). The mixture is then filtered. Triethylamine (0.2 ml, 1.44 mmol, 1.6 eq) is added to the organic layer, and the mixture is again stirred under microwave irradiation, at 120° C. for another 1.5 h. The solvent is then removed under vacuum and the residue diluted with ethyl acetate. The organic layer is washed with water, with a saturated solution of sodium chloride, dried over magnesium sulfate and concentrated under vacuum. The residue is purified over silicagel (eluent: dichloromethane/ethanol/ammonia, gradient from 98:2:0.2 to 96:4:0.4) to give 4,4-dimethyl-2-(4-{3-[(2R)-2-methylpyrrolidin-1-yl]propoxy}phenyl)-4,5-dihydro-1,3-oxazole 15 (60 mg) as a beige powder.

1. filtrationThe mixture is then filtered
2. stirringthe mixture is again stirred under microwave irradiation, at 120° C. for another 1.5 h
3. customThe solvent is then removed under vacuum
4. additionthe residue diluted with ethyl acetate
5. washThe organic layer is washed with water, with a saturated solution of sodium chloride
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under vacuum
8. customThe residue is purified over silicagel (eluent: dichloromethane/ethanol/ammonia, gradient from 98:2:0.2 to 96:4:0.4)