反应详情

To a well stirred suspension of 20.6 g of 4-chlorophenacylamine hydrochloride in 70 ml of benzene and 70 ml of water which was cooled to below 7° C. were added simultaneously 110 ml of 2N NaOH solution and 12.4 g of chloroacetyl chloride dissolved in 30 ml of benzene. After the addition was complete, the reaction mixture was warmed to room temperature and stirred at room temperature for 3 hours. At the end of this period, the formed precipitate was filtered, and the benzene layer was separated. The aqueous layer was extracted twice with 50 ml of benzene. The combined benzene layer was dried over anhydrous sodium sulfate, and evaporated to dryness. The residue together with the precipitate obtained above was combined and recrystallized from ethanol to give 14.1 g (57 percent) of N-(4-chlorophenacyl) chloroacetamide.

1. temperaturewas cooled to below 7° C.
2. additionAfter the addition
3. stirringstirred at room temperature for 3 hours
4. filtrationAt the end of this period, the formed precipitate was filtered
5. customthe benzene layer was separated
6. extractionThe aqueous layer was extracted twice with 50 ml of benzene
7. dry with materialThe combined benzene layer was dried over anhydrous sodium sulfate
8. customevaporated to dryness
9. customThe residue together with the precipitate obtained
10. customrecrystallized from ethanol