Hydrochloric Acid → HCID 178514500, 화합물

HRID 1287181

반응식

HRID 1287181 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 178514500HCID 178514500, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f4cc612eb84048d6b312db1ce99d7ea5
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03984250

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