Ethanol → HCID 178482634、化合物

HRID 1282981ノート

反応式

HRID 1282981 の反応式
[Cl-].[CH3:2][N:3]([CH3:28])[C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[S+:13]=[C:12]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:11]=2)=[CH:6][CH:5]=1.C(O)C.[CH3:32][N:33]([CH3:51])[C:34]1[CH:39]=[CH:38][C:37]([N:40]=[N:41][C:42]2[CH:50]=[CH:49][C:45]([C:46]([O-:48])=[O:47])=[CH:44][CH:43]=2)=[CH:36][CH:35]=1.[Na+]>O>[CH3:32][N:33]([CH3:51])[C:34]1[CH:35]=[CH:36][C:37]([N:40]=[N:41][C:42]2[CH:50]=[CH:49][C:45]([C:46]([O-:48])=[O:47])=[CH:44][CH:43]=2)=[CH:38][CH:39]=1.[CH3:2][N:3]([CH3:28])[C:4]1[CH:5]=[CH:6][C:7]([C:10]2[CH:11]=[C:12]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[S+:13]=[C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:15]=2)=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 702EthanolHCID 23674498Benzoic acid, 4-(2-(4-(dimethylamino)phenyl)diazenyl)-, sodium salt (1:1)HCID 178482633HCID 178482633、化合物

生成物 1

HCID 178482634HCID 178482634、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a hot solution composed of 4.04 g. 4-(4-dimethylaminophenyl)-2,6-diphenylthiapyrylium chloride, 200 mls. water, and 50 mls. ethanol, was added in one portion a solution of sodium 4-(4-dimethylaminophenylazo)benzoate, 3.0 g., in hot water, 150 mls. There was immediate formation of a fine, dark-brown precipitate. The reaction mixture was quickly chilled in ice, and then filtered. The filtrate was a clear, deep orange. The solid was washed with cold water until the washings were only weakly orange. The solid was sucked dry and then a portion of it was dissolved in boiling acetonitrile, filtered hot, and evaporated down. The crystalline solid that came down on cooling the concentrated solution was filtered off and dried in vacuo. This solid was found to contain the above-noted thiapyrylium-azo dye salt.

後処理

  1. temperatureThe reaction mixture was quickly chilled in ice
  2. filtrationfiltered
  3. washThe solid was washed with cold water until the washings
  4. customThe solid was sucked dry
  5. dissolutiona portion of it was dissolved
  6. filtrationfiltered hot
  7. customevaporated down
  8. temperatureon cooling the concentrated solution
  9. filtrationwas filtered off
  10. customdried in vacuo

出典と根拠

ORDレコード
ord-d5846a98ca5d46b092763da42d65d79d
出典データセット
uspto-grants-1976_08
特許番号
US03973962

反応ノート

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