反応 #80265

反応方程式

phenylchloroformate

N-methyldiethanolamine

triethylamine

→

3

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

溶媒

toluene

toluene

反応条件

後処理

1. 1
   その他To a 500 ml three-necked round-bottomed flask equipped with an internal thermometer
2. 2
   温度reflux
3. 3
   workup.ADDITIONcondenser, mechanical stirrer, addition funnel, and argon inlet
4. 4
   温度to maintain the reaction temperature at 35°-45° C
5. 5
   workup.ADDITIONAfter addition
6. 6
   洗浄The cooled mixture is washed with saturated sodium bicarbonate solution (2×200 ml) and water (200 ml)
7. 7
   乾燥The organic phase is dried over MgSO4
8. 8
   ろ過filtered
9. 9
   濃縮concentrated first by rotary evaporation at 50° C. (water aspirator vacuum)

実験手順

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.

出典