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

HRID 2243245
ノート
印刷プレビュー

反応式

HRID 2243245 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 10313229titanium(III) trichloride触媒
HCID 962
Water
溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e8c2ea53ad5a4e639ed3a2cab7a2b6a7
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07674807B2

反応ノート

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