반응 #7433

반응 방정식

N2

Methacrylic acid

t-butyl bromoacetate

DBU

→

t-butyl-2-methacryloyloxyacetate

용매

toluene

반응 조건

후처리

1. 1
   기타equipped with condenser, nitrogen inlet
2. 2
   온도The mixture was cooled to room temperature
3. 3
   기타the salt was removed by filtration
4. 4
   세척The toluene solution was washed with 75 ml saturated NaCl solution and 2×75 ml Dl-water respectively
5. 5
   기타before dried on MgSO4 overnight
6. 6
   여과The solid was filtered out
7. 7
   기타the toluene was removed at rotavap
8. 8
   workup.DISTILLATIONAn oily residue was distilled to a final clear liquid at reduced pressure

실험 절차

Methacrylic acid (8.06 g, 0.10 mole), t-butyl bromoacetate (19.50 g, 0.10 mole) and 1,8-diazabicyclo[5.4.0]undoc-7-ene, DBU, (15.20 g, 0.10 mole) and 150 ml toluene were combined in a 500 ml 3-neck flask equipped with condenser, nitrogen inlet, thermometer and magnetic stirrer bar. The reaction mixture was stirred at room temperature for one hour. The reaction was continued at 90° C. overnight under a blanket of N2 flow. The mixture was cooled to room temperature and the salt was removed by filtration. The toluene solution was washed with 75 ml saturated NaCl solution and 2×75 ml Dl-water respectively before dried on MgSO4 overnight. The solid was filtered out and the toluene was removed at rotavap. An oily residue was distilled to a final clear liquid at reduced pressure.

출처