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Potassium Hydroxide → HCID 178526870, 화합물

HRID 622291
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HRID 622291 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14](Cl)=[C:13]([N+:16]([O-:18])=[O:17])[CH:12]=[N:11]1.[OH-:19].[K+]>CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14]([OH:19])=[C:13]([N+:16]([O-:18])=[O:17])[CH:12]=[N:11]1
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참가 물질

4

반응물 2

HCID 14797Potassium Hydroxide2회HCID 136896085-Chloro-4-nitro-1-(2,4,6-trichlorophenyl)-1H-pyrazole

생성물 1

HCID 178526870HCID 178526870, 화합물수율 49%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3.3 g of 1-(2,4,6-trichlorophenyl)-4-nitro-5-chloropyrazole are suspended in 10 ml of methanol, and 20 ml of 1N methanolic potassium hydroxide solution are added. The mixture is refluxed for 12 hours. In order to achieve complete reaction, a further 10 ml of 1N methanolic potassium hydroxide solution are added to the reaction mixture, which is refluxed for a further 12 hours. For work-up, the mixture is filtered, the solvent is stripped off in vacuo, the residue is taken up in hot water, and the product is precipitated by acidification with 2N hydrochloric acid. After filtering off and drying, 1.5 g (49% of theory) of 1-(2,4,6-trichlorophenyl)-4-nitro-5-hydroxypyrazole of melting point 106°-115° C. are obtained.

후처리

  1. temperatureThe mixture is refluxed for 12 hours
  2. customreaction
  3. temperatureis refluxed for a further 12 hours
  4. filtrationFor work-up, the mixture is filtered
  5. customthe product is precipitated by acidification with 2N hydrochloric acid
  6. filtrationAfter filtering off
  7. customdrying

출처 및 근거

ORD 기록
ord-82ca9ed688b44acfb09b731e9d104103
출처 데이터셋
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04770692

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