反应详情

温度

70 °C

60 g (0.33 mol) of N-formyl-2-methyl-4-nitroaniline were dissolved in 500 ml of dimethylformamide. 184 g (1.33 mol) of potassium carbonate were added, and the resultant solution was warmed to 50° C. 152.8 g (2 mol) of allyl chloride were added dropwise in the course of 50 minutes to the mixture at 50° C. When the alkylation reaction was complete, the resultant reaction mixture was warmed to 70° C. and 350 g of 1 N sodium hydroxide solution were slowly added dropwise. The resultant mixture was stirred at 70° C. for 2.5 hours and subsequently poured into 3 l of ice water. The precipitate was filtered off with suction, washed with water until neutral and subsequently dried at 50° C. under reduced pressure, to give 61 g of N-allyl-2-methyl-4-nitroaniline (yield: 95%), which was recrystallized as described under section 1.4 and then had the same physical chemical properties as the compound prepared in accordance with section 1.4.

1. customWhen the alkylation reaction
2. customthe resultant reaction mixture
3. filtrationThe precipitate was filtered off with suction
4. washwashed with water until neutral and
5. customsubsequently dried at 50° C. under reduced pressure