1-(2-氯乙基)-4-(氯甲基)苯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Vinyl benzene phosphonate was prepared by chloromethylating benzene by the procedure of Kindler, Hansen and Koebk (Ann. Chem. 617, 25, 1958). 1 mole p-(2-chloroethyl)-α-chlorotoluene was heated to 140°-155° C. under N2 and 95 ml triethyl phosphite was added. The mixture was heated for one hour and then diethyl-p-(2-chloroethyl)-benzyl phosphonate was distilled off at 140°-150° C./0.2 torr. The ethyl ester was hydrolysed for two hours using a 2:3 v/v mixture of 48% HBr and formic acid. The product was dehydrochlorinated using potassium ethoxide followed by acidification with HCl. The monomer was then flash distilled using 10-5 torr vacuum at room temperature. The mixture was heated for one hour diethyl-p-(2-chloroethyl)-benzyl phosphonate was distilled off at 140°-150° C./0.2 torr a 2:3 v/v mixture of 48% HBr and formic acid flash distilled at room temperature

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Vinyl benzene phosphonate was prepared by chloromethylating benzene by the procedure of Kindler, Hansen and Koebk (Ann. Chem. 617, 25, 1958). 1 mole p-(2-chloroethyl)-α-chlorotoluene was heated to 140°-155° C. under N2 and 95 ml triethyl phosphite was added. The mixture was heated for one hour and then diethyl-p-(2-chloroethyl)-benzyl phosphonate was distilled off at 140°-150° C./0.2 torr. The ethyl ester was hydrolysed for two hours using a 2:3 v/v mixture of 48% HBr and formic acid. The product was dehydrochlorinated using potassium ethoxide followed by acidification with HCl. The monomer was then flash distilled using 10-5 torr vacuum at room temperature. The mixture was heated for one hour diethyl-p-(2-chloroethyl)-benzyl phosphonate was distilled off at 140°-150° C./0.2 torr a 2:3 v/v mixture of 48% HBr and formic acid flash distilled at room temperature