2,6-Dichloroaniline → 2-(2,6-Dichloroanilino)-1,3,4-trifluoroanthracene-9,10-dione
반응식
[F:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[C:5]([F:18])=[C:4](F)[C:3]=1[F:20].[Cl:21][C:22]1[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[C:23]=1[NH2:24]>>[Cl:21][C:22]1[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[C:23]=1[NH:24][C:4]1[C:3]([F:20])=[C:2]([F:1])[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[C:5]=1[F:18].[Cl:21][C:22]1[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[C:23]=1[NH:24][C:4]1[C:3]([NH:24][C:23]2[C:22]([Cl:21])=[CH:28][CH:27]=[CH:26][C:25]=2[Cl:29])=[C:2]([F:1])[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[C:5]=1[F:18]참가 물질
실험 절차
2 g of 1,2,3,4-Tetrafluoroanthraquinone and 20 g of 2,6-dichloroaniline were charged in a 50 cc, four necked flask and then the reaction was carried out at 230° Cl for about 8 hours. After completion of reaction, 2,6-dichloroaniline was distilled out from the reaction solution, and a column purification thereof using a column with a silica gel was effected to give rise to 1.39 g of 2-(2,6-dichloroanilino)-1,3,4-trifluoroanthraquinone (Dye 10') (yield 46.1 mol %) and 0.78 g of 2,3-bis(2,6-dichloroanilino)-1,4-difluoroanthraquinone (Dye 25') (yield 19.4 mol %). The physical properties of Dye 10' and analytical values defining the compound are tabulated in Table 22 and the physical properties of Dye 25' and analytical values defining the compound are tabulated in Table 23.
후처리
- customwas carried out at 230°
- customfor about 8 hours
- distillationwas distilled out from the reaction solution
- customa column purification
출처 및 근거
- ORD 기록
- ord-daccf23a3d6344268d5b4bd63eaeabea
- 출처 데이터셋
- uspto-grants-1999_10
- 특허 번호
- US05968688
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