反应详情

A mixture of 40 g. (0.184 m.) of the compound of Example I, C., 26.1 g. (0.184 m.) of 2-chloro-5-methylaniline and 500 ml. of ethanol was refluxed with stirring overnight. The reaction mixture was concentrated to dryness in vacuo, and the residue dissolved in 700 m. of MeOH. The insolubles were removed by filtration and the MeOh filtrate concentrated in vacuo to give 24 g. m.p. decomposes 315°-400°C. The crude product was triturated in 500 ml. of MeOH, then oven-dried (100°C) to give m.p. 332°-335°C.

1. additionA mixture of 40 g
2. concentrationThe reaction mixture was concentrated to dryness in vacuo
3. dissolutionthe residue dissolved in 700 m
4. customThe insolubles were removed by filtration
5. concentrationthe MeOh filtrate concentrated in vacuo
6. customto give 24 g
7. customdecomposes 315°-400°C
8. customThe crude product was triturated in 500 ml
9. dry with materialof MeOH, then oven-dried (100°C)
10. customto give m.p. 332°-335°C.