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

HRID 1640098노트

반응식

HRID 1640098 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 10313229titanium(III) trichloride촉매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c8e082579cd34d2f917dc15441dbe3ce
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110689B2

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