反应详情

A solution of 33.4 g of carbomethoxymethylene triphenylphosphine [Helv. Chim. Acta. 40, 1242 (1957)] in 500 ml of dry benzene under nitrogen is treated with 10 g of 2-(bromoacetyl)pyridine and heated at reflux temperature for 2 hours. The reaction mixture is cooled and filtered to remove carbomethoxymethyl triphenylphosphonium bromide. The filtrate, containing triphenylphosphine, is treated with methyl bromoacetate and heated at reflux temperature for 2 hours. Cooling and filtration removes additional phosphonium salt. The filtrate is concentrated in vacuo yielding the title compound.

1. temperatureheated
2. temperatureat reflux temperature for 2 hours
3. temperatureThe reaction mixture is cooled
4. filtrationfiltered
5. customto remove carbomethoxymethyl triphenylphosphonium bromide
6. additionThe filtrate, containing triphenylphosphine
7. additionis treated with methyl bromoacetate
8. temperatureheated
9. temperatureat reflux temperature for 2 hours
10. temperatureCooling
11. filtrationfiltration
12. customremoves additional phosphonium salt
13. concentrationThe filtrate is concentrated in vacuo