反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
31.4 g of 2,6-dimethylanilinoacetic acid methyl amide are dissolved in 250 ml of chlorobenzene. 1.5 ml of dimethyl formamide are added to this solution and the mixture is heated to 110° C. At this temperature 14.3 ml of chloroacetyl chloride are added dropwise with stirring. After 1 1/2 hours the evolution of HCl has virtually ceased. The reaction mixture is allowed to cool and concentrated in a rotary evaporator to leave as residue a blackish-brown oil which is crystallised from ethyl acetate with the addition of animal charcoal. Yield: 22.4 g of N-methyl-[N'-(2,6-dimethylphenyl)-N'-chloroacetylamino]-acetamide (m.p. 140° C-142° C). N,N-dimethyl-(N'-(2,6-dimethylphenyl)-N'-chloroacetylamino]-acetamide was obtained in analogous manner; m.p. 74°-76° C (from ether).
WORKUP
后处理
- customAfter 1 1/2 hours
- temperatureto cool
- concentrationconcentrated in a rotary evaporator
- customto leave as residue a blackish-brown oil which
- customis crystallised from ethyl acetate with the addition of animal charcoal