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Acetone → 1-(3-methyl-4-aminobenzyl)-3,5-bis(trifluoromethyl)-1H-pyrazole

HRID 2243245
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HRID 2243245 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[N+:22]([O-])=O)[CH2:5][N:6]1[C:10]([C:11]([F:14])([F:13])[F:12])=[CH:9][C:8]([C:15]([F:18])([F:17])[F:16])=[N:7]1.C([O-])(=O)C.[NH4+].CC(C)=O>[Cl-].[Cl-].[Cl-].[Ti+3].O>[CH3:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[NH2:22])[CH2:5][N:6]1[C:10]([C:11]([F:12])([F:13])[F:14])=[CH:9][C:8]([C:15]([F:18])([F:17])[F:16])=[N:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 180AcetoneHCID 517165Ammonium AcetateHCID 592104091-(3-methyl-4-nitrobenzyl)-3,5-bis(trifluoromethyl)-1H-pyrazole

생성물 1

HCID 592103951-(3-methyl-4-aminobenzyl)-3,5-bis(trifluoromethyl)-1H-pyrazole수율 92.9%

시약·촉매·용매 2

HCID 10313229titanium(III) trichloride촉매
HCID 962
Water
용매

실험 절차

To a mixture of 1-(3-methyl-4-nitrobenzyl)-3,5-bis(trifluoromethyl)-1H-pyrazole (1.4 g), ammonium acetate (30.5 g), acetone (60 ml) and water (30 ml), 20% aqueous solution of titanium trichloride (27.5 g) was added at room temperature and the mixture was stirred at room temperature for 12 hours. After finishing the reaction, the mixture was extracted with ethyl acetate, washed with saturated aqueous solution of sodium chloride and dried with anhydrous sodium sulfate. After distilling off the solvent, the obtained residue was purified by silica gel column chromatography to obtain 1-(3-methyl-4-aminobenzyl)-3,5-bis(trifluoromethyl)-1H-pyrazole (1.19 g).

후처리

  1. additionwas added at room temperature
  2. customthe reaction
  3. extractionthe mixture was extracted with ethyl acetate
  4. washwashed with saturated aqueous solution of sodium chloride
  5. dry with materialdried with anhydrous sodium sulfate
  6. distillationAfter distilling off the solvent
  7. customthe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-e8c2ea53ad5a4e639ed3a2cab7a2b6a7
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07674807B2

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