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Thionyl Chloride → 4-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonyl chloride

HRID 1680384
ノート
印刷プレビュー

反応式

HRID 1680384 の反応式
[C:1]([O:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([S:20](O)(=[O:22])=[O:21])=[CH:12][C:11]=1[N:24]=[N:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:34])=O>CN(C)C=O>[C:1]([O:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([S:20]([Cl:34])(=[O:22])=[O:21])=[CH:12][C:11]=1[N:24]=[N:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 234561594-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonic acid

生成物 1

HCID 234561604-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonyl chloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonic acid (70 g) was added to thionyl chloride (300 ml). Dimethylformamide (30 ml) was added in portions while the reaction mixture was being stirred. After 1 hour the starting material was all in solution. The reaction mixture was poured into a large quantity of ice after a further 4 hours' stirring. The product was filtered off and dissolved in chloroform. The chloroform layer was shaken with water to destroy any remaining thionyl chloride and dried over magnesium sulfate.

後処理

  1. additionThe reaction mixture was poured into a large quantity of ice after a further 4 hours'
  2. stirringstirring
  3. filtrationThe product was filtered off
  4. dissolutiondissolved in chloroform
  5. stirringThe chloroform layer was shaken with water
  6. customto destroy any remaining thionyl chloride
  7. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-aea4bbe39c694b5bb462fd1092a8af76
出典データセット
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04273706

反応ノート

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