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

HRID 1975960ノート

反応式

HRID 1975960 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-eece56e977e84d8884747d6be26836bf
出典データセット
uspto-grants-2001_05
特許番号
US06225316B1

反応ノート

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