反応 #7433

反応方程式

N2

Methacrylic acid

t-butyl bromoacetate

DBU

→

t-butyl-2-methacryloyloxyacetate

溶媒

toluene

反応条件

後処理

1. 1
   その他equipped with condenser, nitrogen inlet
2. 2
   温度The mixture was cooled to room temperature
3. 3
   その他the salt was removed by filtration
4. 4
   洗浄The toluene solution was washed with 75 ml saturated NaCl solution and 2×75 ml Dl-water respectively
5. 5
   その他before dried on MgSO4 overnight
6. 6
   ろ過The solid was filtered out
7. 7
   その他the toluene was removed at rotavap
8. 8
   workup.DISTILLATIONAn oily residue was distilled to a final clear liquid at reduced pressure

実験手順

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.

出典