Hydrochloric Acid → HCID 178514500、化合物

HRID 1287181

反応式

HRID 1287181 の反応式
[N+:1](=[C:3]1[CH:12]=[CH:11][C:10]2[C:9]([S:13](Cl)(=[O:15])=[O:14])=[CH:8][CH:7]=[CH:6][C:5]=2[C:4]1=[O:17])=[N-:2].[K].[OH:19][C:20]1[CH:25]=[CH:24][C:23]([N:26]=[N+:27]=[N-:28])=[CH:22][CH:21]=1.Cl>O1CCOCC1.O>[N+:1](=[C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[S:13]([O:19][C:20]2[CH:25]=[CH:24][C:23]([N:26]=[N+:27]=[N-:28])=[CH:22][CH:21]=2)(=[O:15])=[O:14])[C:4]1=[O:17])=[N-:2]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 5462222PotassiumHCID 116223404-AzidophenolHCID 1363787716-Diazo-5,6-dihydro-5-oxo-1-naphthalenesulfonyl chloride

生成物 1

HCID 178514500HCID 178514500、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒2 回

実験手順

1,2-Dihydro-2-diazo-1-oxo-naphthalene-5-sulfonyl chloride (2.2 grams) is dissolved in dioxane (16 mls.) and the potassium salt of 4-hydroxyphenylazide (1.6 grams) in a mixture of water (4 ml.) and dioxane (4 ml.) is added gradually over a period of 10 minutes with stirring. The mixture is then stirred at room temperature (22°C) for 30 minutes to complete the reaction and then diluted with water (60 ml.) containing 3N hydrochloric acid (8 ml.). An oil separates out which solidifies on standing. The product is then collected and dried (2.5 grams). It is dissolved in benzene treated with carbon and filtered. Addition of 60°-80° pet. ether to the filtrate yields Compound 1. (1.7 grams) m.p. 136°-7° with decomposition.

後処理

  1. additionis added gradually over a period of 10 minutes
  2. stirringThe mixture is then stirred at room temperature (22°C) for 30 minutes
  3. customthe reaction
  4. customThe product is then collected
  5. customdried (2.5 grams)
  6. dissolutionIt is dissolved in benzene
  7. additiontreated with carbon
  8. filtrationfiltered
  9. additionAddition of 60°-80° pet. ether to the filtrate

出典と根拠

ORDレコード
ord-f4cc612eb84048d6b312db1ce99d7ea5
出典データセット
uspto-grants-1976_10
特許番号
US03984250

関連ノート

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