1,6-Cleve's acid → HCID 12094653、化合物

HRID 480669

反応式

HRID 480669 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([S:12]([OH:15])(=[O:14])=[O:13])=[CH:7]2.[N+:16]([C:19]1[CH:20]=[C:21]([C:28](Cl)=[O:29])[CH:22]=[C:23]([C:25](Cl)=[O:26])[CH:24]=1)([O-:18])=[O:17]>N1C=CC=CC=1.O1CCOCC1.C(Cl)(Cl)Cl>[N+:16]([C:19]1[CH:20]=[C:21]([C:28]([NH:1][C:2]2[CH:11]=[CH:10][CH:9]=[C:8]3[C:3]=2[CH:4]=[CH:5][C:6]([S:12]([OH:15])(=[O:13])=[O:14])=[CH:7]3)=[O:29])[CH:22]=[C:23]([C:25](=[O:26])[NH:1][C:2]2[C:3]3[C:8](=[CH:7][C:6]([S:12]([OH:15])(=[O:13])=[O:14])=[CH:5][CH:4]=3)[CH:9]=[CH:10][CH:11]=2)[CH:24]=1)([O-:18])=[O:17]

参加物

6

反応物 2

HCID 84081,6-Cleve's acidHCID 834515-Nitroisophthaloyl chloride

生成物 1

HCID 12094653HCID 12094653、化合物

試薬・触媒・溶媒 3

HCID 1049Pyridine溶媒HCID 6212Chloroform溶媒HCID 312751,4-Dioxane溶媒

実験手順

22.33 g (0.10 mol) of 5-amino-2-naphthalenesulfonic acid was suspended in 150 mL of pyridine and added to the above di-acid chloride in 50 mL (50:50) of dioxane and CHCl3 under vigorous stirring for 1-2 hrs. The crude product was precipitated with dioxane. The oily product was collected on a Büchner funnel. The brown colored oily product was dissolved in 500 mL water, then allowed to precipitate out over 30 min. The solid material was collected using filtration. It yielded 16.2 g.

後処理

  1. customThe crude product was precipitated with dioxane
  2. customThe oily product was collected on a Büchner funnel
  3. dissolutionThe brown colored oily product was dissolved in 500 mL water
  4. customto precipitate out over 30 min
  5. customThe solid material was collected
  6. filtrationfiltration
  7. customIt yielded 16.2 g

出典と根拠

ORDレコード
ord-5e3368348bc7428f8858fabd35c3d318
出典データセット
uspto-grants-2003_11
特許番号
US06653321B1

関連ノート

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