反应详情

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.

1. customequipped with condenser, nitrogen inlet
2. temperatureThe mixture was cooled to room temperature
3. customthe salt was removed by filtration
4. washThe toluene solution was washed with 75 ml saturated NaCl solution and 2×75 ml Dl-water respectively
5. custombefore dried on MgSO4 overnight
6. filtrationThe solid was filtered out
7. customthe toluene was removed at rotavap
8. distillationAn oily residue was distilled to a final clear liquid at reduced pressure