Acetone → 4-(3,5-Bis-trifluoromethyl-benzyl)-2-methylaniline

HRID 1640098ノート

反応式

HRID 1640098 の反応式
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[C:5]([CH:17]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:19]=1)[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[C:9]([CH3:16])[CH:8]=1.C([O-])(=O)C.[NH4+].CC(C)=O>[Cl-].[Cl-].[Cl-].[Ti+3].O>[F:1][C:2]([F:24])([F:25])[C:3]1[CH:4]=[C:5]([CH:17]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:19]=1)[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH2:13])=[C:9]([CH3:16])[CH:8]=1

参加物

6

反応物 3

HCID 180AcetoneHCID 517165Ammonium AcetateHCID 592295044-(3,5-Bis-trifluoromethyl-benzyl)-2-methylnitrobenzene

生成物 1

HCID 120027444-(3,5-Bis-trifluoromethyl-benzyl)-2-methylaniline収率 54.5%

試薬・触媒・溶媒 2

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

実験手順

A solution of 20% titanium trichloride (8.4 g) was added to a mixture of 4-(3,5-bis-trifluoromethyl-benzyl)-2-methyl-nitrobenzene (0.44 g), ammonium acetate (9.3 g), acetone (20 ml) and water (10 ml) at room temperature and stirred for 12 hours. After the reaction, the reaction solution was extracted with ethyl acetate and washed with a saturated sodium bicarbonate solution and a saturated salt solution and then dried over anhydrous magnesium sulfate. After distilling the solvent off, the resultant residue was purified by silica gel column chromatography to obtain 4-(3,5-bis-trifluoromethyl-benzyl)-2-methylaniline (0.22 g).

後処理

  1. customAfter the reaction
  2. extractionthe reaction solution was extracted with ethyl acetate
  3. washwashed with a saturated sodium bicarbonate solution
  4. dry with materiala saturated salt solution and then dried over anhydrous magnesium sulfate
  5. distillationAfter distilling the solvent off, the resultant residue
  6. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-c8e082579cd34d2f917dc15441dbe3ce
出典データセット
uspto-grants-2012_02
特許番号
US08110689B2

反応ノート

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