反应详情

To a three necked 100 mL round bottom flask fitted with a argon inlet, dropping funnel, distillation unit and magnetic needle, was added 7.7 mmoles of tetrabutylammonium hydroxide (20% solution in toluene/methanol) in 40 mL of dry toluene and heated to +75° C. to +85° C. Diethylphenylmalonate (9.3 mmoles) was slowly added. Simultaneously an azeotrope of toluene-water was distilled out slowly over a period of 3 hours. After all toluene had distilled over, the flask was cooled to room temperature slowly. A solid product separated out, which was repeatedly washed with dry hexane. The initiator (tetra-n-butyl ammonium diethylphenyl malonate) thus formed was dried in vacuum and stored at room temperature under nitrogen or argon.

1. customTo a three necked 100 mL round bottom flask fitted with a argon inlet
2. distillationdistillation unit and magnetic needle
3. temperatureheated to +75° C. to +85° C
4. distillationSimultaneously an azeotrope of toluene-water was distilled out slowly over a period of 3 hours
5. distillationAfter all toluene had distilled over, the flask
6. customA solid product separated out
7. washwhich was repeatedly washed with dry hexane