ethylidene(triphenyl)-lambda5-phosphane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a diethyl ether solution of ethylidenetriphenylphosphorane prepared in the usual way from 800 g. of ethyltriphenylphosphonium bromide, 400 g. of ethyl 3,4-dimethoxyphenylglyoxylate in 600 ml. of ether are added dropwise. After refluxing for 4-5 hours, the solvent is evaporated and substituted with tetrahydrofuran. The mixture is then heated for 36 hours and then evaporated to dryness and the residue is extracted with diethyl ether in a Soxhlet apparatus giving 150 g. of the title compound. Pursuant to this procedure, the following other α-arylcrotonate starting materials are prepared: After refluxing for 4-5 hours the solvent is evaporated The mixture is then heated for 36 hours evaporated to dryness the residue is extracted with diethyl ether in a Soxhlet apparatus giving 150 g

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a diethyl ether solution of ethylidenetriphenylphosphorane prepared in the usual way from 800 g. of ethyltriphenylphosphonium bromide, 400 g. of ethyl 3,4-dimethoxyphenylglyoxylate in 600 ml. of ether are added dropwise. After refluxing for 4-5 hours, the solvent is evaporated and substituted with tetrahydrofuran. The mixture is then heated for 36 hours and then evaporated to dryness and the residue is extracted with diethyl ether in a Soxhlet apparatus giving 150 g. of the title compound. Pursuant to this procedure, the following other α-arylcrotonate starting materials are prepared: After refluxing for 4-5 hours the solvent is evaporated The mixture is then heated for 36 hours evaporated to dryness the residue is extracted with diethyl ether in a Soxhlet apparatus giving 150 g

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a diethyl ether solution of ethylidenetriphenylphosphorane prepared in the usual way from 800 g. of ethyltriphenylphosphonium bromide, 400 g. of ethyl 3,4-dimethoxyphenylglyoxylate in 600 ml. of ether are added dropwise. After refluxing for 4-5 hours, the solvent is evaporated and substituted with tetrahydrofuran. The mixture is then heated for 36 hours and then evaporated to dryness and the residue is extracted with diethyl ether in a Soxhlet apparatus giving 150 g. of the title compound. Pursuant to this procedure, the following other α-arylcrotonate starting materials are prepared: After refluxing for 4-5 hours the solvent is evaporated The mixture is then heated for 36 hours evaporated to dryness the residue is extracted with diethyl ether in a Soxhlet apparatus giving 150 g