反应详情

A mixture of 38.6 g (0.3 mole) of 4-chlorophenol, 70 g (0.36 mole) of diethylchloromalonate and 69.1 g (0.5 mole) of anhydrous potassium carbonate in 750 ml of acetone was heated at reflux for 48 hr, cooled, filtered and the filtrate concentrated. The residue was diluted with 250 ml of ethyl ether and was washed successively with two 100 ml portions of a 1% NaOH solution, once with H2O and once with brine, dried (sodium sulfate) and concentrated to give an oil which gradually crystallized. The solid was triturated with petroleum ether (30°-60° C.), collected by filtration and dried to yield 72.6 g (84%) of white solid. An analytical sample, mp 43.5°-45° C. (lit. mp 58°-60° C.), was recrystallized from petroleum ether (60°-110° C.).

1. temperaturewas heated
2. temperatureat reflux for 48 hr
3. temperaturecooled
4. filtrationfiltered
5. concentrationthe filtrate concentrated
6. additionThe residue was diluted with 250 ml of ethyl ether
7. washwas washed successively with two 100 ml portions of a 1% NaOH solution, once with H2O and once with brine
8. dry with materialdried (sodium sulfate)
9. concentrationconcentrated
10. customto give an oil which
11. customgradually crystallized
12. customThe solid was triturated with petroleum ether (30°-60° C.)
13. filtrationcollected by filtration
14. customdried