3,5-Bis(trifluoromethyl)benzylamine → n-(3,5-Bis-trifluoromethyl-benzyl)-3-o-tolyl-isonicotinamide

HRID 1975960노트

반응식

HRID 1975960 반응식
[C:1]1([CH3:16])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[CH:15]=[N:14][CH:13]=[CH:12][C:8]=1[C:9]([OH:11])=O.[F:17][C:18]([F:32])([F:31])[C:19]1[CH:20]=[C:21]([CH:24]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:26]=1)[CH2:22][NH2:23].Cl.CN(C)CCCN=C=NCC>ClCCl>[F:17][C:18]([F:31])([F:32])[C:19]1[CH:20]=[C:21]([CH:24]=[C:25]([C:27]([F:30])([F:28])[F:29])[CH:26]=1)[CH2:22][NH:23][C:9](=[O:11])[C:8]1[CH:12]=[CH:13][N:14]=[CH:15][C:7]=1[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[CH3:16]

참가 물질

5

반응물 3

HCID 5210993,5-Bis(trifluoromethyl)benzylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 220000663-(2-Methylphenyl)-4-pyridinecarboxylic acid

생성물 1

HCID 22000068n-(3,5-Bis-trifluoromethyl-benzyl)-3-o-tolyl-isonicotinamide수율 51%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.28 g (1.17 mol) 3-o-tolyl-isonicotinic acid and 0.34 g (1.40 mmol) 3,5-bis(trifluoromethyl)benzylamine in 10 ml dichloromethane 0.38 ml N-methylmorpholine and 0.27 g (1.40 mmol) N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimide hydrochloride were added and the mixture stirred for 12 h. The phases were separated, the water phase extracted with three portions of dichloromethane. The combined organic phases were dried (magnesium sulfate) and evaporated. Chromatography of the residue afforded 0.26 g (51%) of the title compound as a colorless oil.

후처리

  1. customThe phases were separated
  2. extractionthe water phase extracted with three portions of dichloromethane
  3. dry with materialThe combined organic phases were dried (magnesium sulfate)
  4. customevaporated

출처 및 근거

ORD 기록
ord-eece56e977e84d8884747d6be26836bf
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06225316B1

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