反应详情

A mixture of 2-benzylthio-4,5-dihydro-1H-imidazole (15.4 grams, 0.08 mole), 5-(1-methylethyl)-1,3-cyclohexanedione (12.3 grams, 0.08 mole) and 0.11 gram of DABCO is heated at 115°-120° C., with stirring, for a period of 7.1 hours. The cooled residue is dissolved in dichloromethane and the solution extracted with three portions of 3N sodium hydroxide, then with four portions of 3N hydrochloric acid. The organic phase is then dried over magnesium sulfate and evaporated, to give 15.31 grams of crude product as a yellow solid. The material is recrystallized twice from toluene and once from ethyl acetate, to give 2.58 grams of product, m.p. 223°-225° C.

1. temperatureis heated at 115°-120° C.
2. extractionthe solution extracted with three portions of 3N sodium hydroxide
3. dry with materialThe organic phase is then dried over magnesium sulfate
4. customevaporated
5. customto give 15.31 grams of crude product as a yellow solid
6. customThe material is recrystallized twice from toluene and once from ethyl acetate