2,3,5,6-Tetrachloroaniline → HCID 21836024、化合物

HRID 1739621ノート

反応式

HRID 1739621 の反応式
[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[C:28]([Cl:29])=[CH:27][C:26]([Cl:30])=[C:25]([Cl:31])[C:23]=1[NH2:24]>>[Cl:21][C:22]1[C:28]([Cl:29])=[CH:27][C:26]([Cl:30])=[C:25]([Cl:31])[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[C:28]([Cl:29])=[CH:27][C:26]([Cl:30])=[C:25]([Cl:31])[C:23]=1[NH:24][C:4]1[C:3]([NH:24][C:23]2[C:25]([Cl:31])=[C:26]([Cl:30])[CH:27]=[C:28]([Cl:29])[C:22]=2[Cl:21])=[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]

参加物

4

反応物 2

HCID 189982,3,5,6-Tetrachloroaniline2 回HCID 2833793HCID 2833793、化合物

生成物 2

HCID 21836024HCID 21836024、化合物HCID 21836049HCID 21836049、化合物

実験手順

2 g of 1,2,3,4-Tetrafluoroanthraquinone and 30 g of 2,3,5,6-tetrachloroaniline were charged in a 50 cc, four necked flask and then the reaction was carried out at 210° C. for about 10 hours. After completion of reaction, 2,3,5,6-tetrachloroaniline 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 0.62 g of 2-(2,3,5,6-tetrachloroanilino)-1,3,4-trifluoroanthraquinone (Dye 11') (yield 17.8 mol %) and 0.53 g of 2,3-bis(2,3,5,6-tetrachloroanilino)-1,4-difluoroanthraquinone (Dye 27') (yield 10.6 mol %). The physical properties of Dye 11' and analytical values defining the compound are tabulated in Table 22 and the physical properties of Dye 27' and analytical values defining the compound are tabulated in Table 23.

後処理

  1. distillationwas distilled out from the reaction solution
  2. customa column purification

出典と根拠

ORDレコード
ord-bafffc5473504cdd8e9d58c8e0fd27d3
出典データセット
uspto-grants-1999_10
特許番号
US05968688

反応ノート

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