反应详情

To a 500 ml three-necked round-bottomed flask equipped with an internal thermometer, reflux condenser, mechanical stirrer, addition funnel, and argon inlet are added N,N-dimethylethanolamine (25.00 g, 0.281 mol), toluene (200 ml), and triethylamine (31.21 g, 0.309 mol). The mixture is treated with a solution of phenylchloroformate (43.91 g, 0.281 mol) dissolved in 50 ml of toluene over 15 min. After addition is complete, the mixture is heated to reflux for 3 h. The cooled mixture is washed with saturated sodium bicarbonate solution (2×100 ml) and water (100 ml). The organic phase is dried over MgSO4, filtered, and concentrated first by rotary evaporation at 50° C. (water aspirator vacuum) and then at 60° C. (0.05 mmHg) in a Kugelrohr oven to give 8 as a light yellow oil, 49.93 g (85%) that crystallizes on standing.

1. customTo a 500 ml three-necked round-bottomed flask equipped with an internal thermometer
2. temperaturereflux
3. additioncondenser, mechanical stirrer, addition funnel, and argon inlet
4. additionAfter addition
5. temperaturethe mixture is heated
6. temperatureto reflux for 3 h
7. washThe cooled mixture is washed with saturated sodium bicarbonate solution (2×100 ml) and water (100 ml)
8. dry with materialThe organic phase is dried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated first by rotary evaporation at 50° C. (water aspirator vacuum)