Ammonia → HCID 20393029、化合物

反応式

Cl[C:2]1[N:10]=[C:9]([CH3:11])[CH:8]=[C:7]([CH3:12])[C:3]=1[C:4]([OH:6])=O.[CH3:13][C:14]1[C:19]([CH3:20])=[CH:18][C:17]([NH2:21])=[C:16]([NH2:22])[CH:15]=1.N>S1(CCCC1)(=O)=O>[CH3:11][C:9]1[CH:8]=[C:7]([CH3:12])[C:3]2[C:4](=[O:6])[NH:22][C:16]3[CH:15]=[C:14]([CH3:13])[C:19]([CH3:20])=[CH:18][C:17]=3[NH:21][C:2]=2[N:10]=1

参加物

反応条件

温度: 220 °C

実験手順

A mixture consisting of 52.0 gm of 2-chloro-4,6-dimethyl-nicotinic acid, 38.0 gm of 4,5-dimethyl-o-phenylenediamine and 150 ml of sulfolane was heated on an oil bath at 220° C. After 45 minutes the mixture was allowed to cool to 100° C. and was then poured over ice. After neutralization with ammonia and standing for several hours the precipitate which had formed was suction-filtered off and admixed with dilute acetic acid. The mixture was suction-filtered after one hour, and the filter cake was recrystallized from aqueous 80% acetic acid, yielding 34% of theory of the compound named in the heading, which had a melting point of 264°-268° C.