反应详情

A mixture of 2,3-diamino-4-methoxytoluene [prepared by hydrogenation of 4-methoxy-2,3-dinitrotoluene (7.5 g) over 10% palladium-carbon (2.5 g) in ethanol] and 4-chlorophenylacetic acid (23 g) was heated at 130°-150° C. for 4.5 h under nitrogen. The mixture was cooled, dissolved in chloroform, washed with 10% sodium carbonate solution, then with water, dried (Na2SO4) and evaporated to dryness in vacuo. The product was recrystallized from chloroform-pentane to afford the title compound, (5.75 g), m.p. 195°-197° C.

1. temperaturewas heated at 130°-150° C. for 4.5 h under nitrogen
2. temperatureThe mixture was cooled
3. washwashed with 10% sodium carbonate solution
4. dry with materialwith water, dried (Na2SO4)
5. customevaporated to dryness in vacuo
6. customThe product was recrystallized from chloroform-pentane