反应详情

With stirring, 816 mg (6.43 mmol) of 1,3-dichloroacetone and 1000 mg (6.43 mmol) of p-chlorobenzamide are heated at +135° C. for 1 h. After cooling to RT, 1.6 ml of conc. sulphuric acid are added, and the mixture is stirred at RT for a further 5 min. The entire mixture is then poured onto 50 ml of ice. A precipitate is formed which is filtered off with suction, dried under high vacuum and then purified chromatographically on silica gel 60 (mobile phase: gradient cyclohexane/ethyl acetate 20:1→5:1).

1. stirringthe mixture is stirred at RT for a further 5 min
2. customA precipitate is formed which
3. filtrationis filtered off with suction
4. customdried under high vacuum
5. custompurified chromatographically on silica gel 60 (mobile phase: gradient cyclohexane/ethyl acetate 20:1→5:1)