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Hydrazine hydrate (1:1) → HCID 940183, 화합물

HRID 1498928
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HRID 1498928 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:10]=[C:11]([C:14]([OH:16])=O)[NH:12][N:13]=1.O.[NH2:18][NH2:19]>CO.S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:10]=[C:11]([C:14]([NH:18][NH2:19])=[O:16])[NH:12][N:13]=1
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 9451245-(2,4-dichlorophenyl)-1H-pyrazole-3-carboxylic acid

생성물 1

HCID 940183HCID 940183, 화합물수율 87%

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 887Methanol용매

실험 절차

In methanol (20 ml), 5-(2,4-dichlorophenyl)-2H-pyrazole-3-carboxylic acid (1.00 g) was dissolved, and 6 drops of concentrated sulfuric acid was added thereto. The mixture was heated under reflux for 19 hours. After the mixture was allowed to cool, hydrazine monohydrate (0.97 g) was added to the mixture, and the resulting mixture was heated under reflux for 16 hours. The mixture was concentrated under a reduced pressure, and water was added thereto. The precipitated crystal was separated by filtration, washed with water, and dried to give the title compound (912 mg, 87%) as a white powder.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 19 hours
  3. temperatureto cool
  4. temperaturethe resulting mixture was heated
  5. temperatureunder reflux for 16 hours
  6. concentrationThe mixture was concentrated under a reduced pressure, and water
  7. additionwas added
  8. customThe precipitated crystal was separated by filtration
  9. washwashed with water
  10. customdried

출처 및 근거

ORD 기록
ord-4818ad5150814f3fb1109d6d6d20937c
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200008B2

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