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Formic Acid → HCID 19786355, 화합물

HRID 1656891
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HRID 1656891 반응식
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([O:13][C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[CH:4][C:3]=1[C:19]#N.C(O)=[O:22]>[Ni]>[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([O:13][C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[CH:4][C:3]=1[CH:19]=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 284Formic AcidHCID 135618335-Amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole

생성물 1

HCID 19786355HCID 19786355, 화합물수율 62%

시약·촉매·용매 1

HCID 935Nickel촉매

실험 절차

12 g (0.042 mol) of 5-amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole are boiled under reflux with 5 g of Raney nickel in 50 ml of 75% strength aqueous formic acid for 1 hour; the still warm solution is filtered under suction, the residue is rinsed with water, the filtrate is extracted several times with ether, and the combined ether phases are washed with saturated sodium bicarbonate solution, dried over sodium sulphate and evaporated down in vacuo. 8.0 g (62% of theory) of 5-amino-1-(2-chloro-4-trifluoromethoxy-phenyl)-4-formylpyrazole are obtained in the form of an oil.

후처리

  1. filtrationthe still warm solution is filtered under suction
  2. washthe residue is rinsed with water
  3. extractionthe filtrate is extracted several times with ether
  4. washthe combined ether phases are washed with saturated sodium bicarbonate solution
  5. dry with materialdried over sodium sulphate
  6. customevaporated down in vacuo

출처 및 근거

ORD 기록
ord-26cf8a5d8b93474dab56a66f3dfca75b
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05256634

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