Pyridine → N-Methoxy-N-methyl-4-(trifluoromethyl)benzamide

HRID 585973

反応式

HRID 585973 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1.Cl.[CH3:15][NH:16][O:17][CH3:18].N1C=CC=CC=1>C(Cl)Cl.C(OCC)C>[CH3:18][O:17][N:16]([CH3:15])[C:7](=[O:8])[C:6]1[CH:10]=[CH:11][C:3]([C:2]([F:13])([F:12])[F:1])=[CH:4][CH:5]=1

参加物

6

反応物 3

HCID 1049PyridineHCID 676074-(Trifluoromethyl)benzoyl chlorideHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)

生成物 1

HCID 14069348N-Methoxy-N-methyl-4-(trifluoromethyl)benzamide

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

4-(Trifluoromethyl)benzoyl chloride (5.0 g, 23.9 mmol) and N,O-dimethylhydroxylamine hydrochloride (2.55 g, 26.3 mmol, 1.1 eq.) were combined in CH2Cl2 (200 mL) at 0° C. and treated with pyridine (4.3 mL, 52.6 mmol). After stirring for 2 hours, the mixture was allowed to attain ambient temperature, diluted with diethyl ether and washed with water, aqueous HCl, and water. the organic phase was separated and concentrated to provide the title compound which was used directly in the next step. 1H NMR (300 MHz, d6-DMSO) 7.90 (m, 4H), 3.52 (s, 3H), 3.28 (s, 3H); MS (DCI/NH3) m/e 234 (M+H)+.

後処理

  1. customto attain ambient temperature
  2. washwashed with water, aqueous HCl, and water
  3. customthe organic phase was separated
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-ff9ef132d9564af882d03ceee67b3dc2
出典データセット
uspto-grants-2005_08
特許番号
US06933311B2

関連ノート

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