反应详情

33.6 g (114.3 mmol) of phosphonoacetic acid triethyl ester is introduced into 148 ml of tetrahydrofuran. At 0° C., 79.7 ml of a 2 M solution of LDA in THF/heptane/ethylbenzene is added in drops (1½ hours). After one hour of stirring, 24.3 g (136.34 mmol) of 2-(3-methoxyphenyl)-2-methylpropanal, dissolved in 130 ml of tetrahydrofuran, is added in drops at 0° C. After five days of stirring at room temperature, the reaction mixture is poured into 250 ml of dilute ammonium chloride solution and extracted twice with 400 ml each of diethyl ether. The combined organic extracts are treated as usual, and the residue that is obtained is chromatographed on silica gel (mobile solvent ethyl acetate/hexane). 27.2 g (80.4%) of the desired compound is isolated.

1. additionis added in drops at 0° C
2. stirringAfter five days of stirring at room temperature
3. extractionextracted twice with 400 ml each of diethyl ether
4. additionThe combined organic extracts are treated as usual, and the residue that
5. customis obtained
6. customis chromatographed on silica gel (mobile solvent ethyl acetate/hexane)