반응 #80265

반응 방정식

phenylchloroformate

N-methyldiethanolamine

triethylamine

→

3

N,N-Bis[2-((phenoxycarbonyl)oxy)ethyl]-N-methylamine

용매

toluene

toluene

반응 조건

후처리

1. 1
   기타To a 500 ml three-necked round-bottomed flask equipped with an internal thermometer
2. 2
   온도reflux
3. 3
   workup.ADDITIONcondenser, mechanical stirrer, addition funnel, and argon inlet
4. 4
   온도to maintain the reaction temperature at 35°-45° C
5. 5
   workup.ADDITIONAfter addition
6. 6
   세척The cooled mixture is washed with saturated sodium bicarbonate solution (2×200 ml) and water (200 ml)
7. 7
   건조The organic phase is dried over MgSO4
8. 8
   여과filtered
9. 9
   농축concentrated first by rotary evaporation at 50° C. (water aspirator vacuum)

실험 절차

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-methyldiethanolamine (20.00 g, 0.168 mol), toluene (200 ml), and triethylamine (37.36 g, 0.369 mol). The minute is treated with a solution of phenylchloroformate (52.56 g, 0.336 mol dissolved in 50 ml of toluene so as to maintain the reaction temperature at 35°-45° C. After addition is complete, the mixture is heated at 45° C. for an additional 1.5 h. The cooled mixture is washed with saturated sodium bicarbonate solution (2×200 ml) and water (200 ml). The organic phase is dried over MgSO4, filtered, and concentrated first by rotary evaporation at 50° C. (water aspirator vacuum) and then at 80° C. (0.02 mmHg) in a Kugelrohr oven to give 3 as a light yellow oil, 55.65 g (92%) that crystallizes on standing.

출처