Benzene → N-(1-methoxy-2,2,2-trifluoroethyl)-4-methoxy-6-{3-(trifluoromethyl)phenoxy}-2-pyridine carboxamide

HRID 1250500ノート

反応式

HRID 1250500 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)[N:6]=[C:5]([C:20]([NH2:22])=[O:21])[CH:4]=1.O.[F:24][C:25]([F:29])([F:28])[CH:26]=[O:27].[CH:30]1C=CC=CC=1>>[CH3:30][O:27][CH:26]([NH:22][C:20]([C:5]1[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:18])([F:19])[F:17])[CH:11]=2)[N:6]=1)=[O:21])[C:25]([F:29])([F:28])[F:24]

参加物

4

反応物 3

HCID 241BenzeneHCID 27813662,2,2-Trifluoroacetaldehyde hydrateHCID 183262294-Methoxy-6-{3-(trifluoromethyl)phenoxy}-2-pyridine carboxamide

生成物 1

HCID 18326218N-(1-methoxy-2,2,2-trifluoroethyl)-4-methoxy-6-{3-(trifluoromethyl)phenoxy}-2-pyridine carboxamide

実験手順

4-methoxy-6-{3-(trifluoromethyl)phenoxy}-2-pyridine carboxamide was dissolved in benzene and mixed with 0.36 g (0.0026×1.2 mol) of trifluoroacetaldehyde hydrate, followed by treating the obtained solution under reflux for about 5 hours. The reaction solution was concentrated and then distributed in ethyl acetate-saturated sodium bicarbonate water, followed by washing with saturated brine. The organic phase of the obtained solution was dried with anhydrous sodium sulfate, concentrated and purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

後処理

  1. additionby treating the obtained solution
  2. temperatureunder reflux for about 5 hours
  3. concentrationThe reaction solution was concentrated
  4. washby washing with saturated brine
  5. dry with materialThe organic phase of the obtained solution was dried with anhydrous sodium sulfate
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-e645bd9b7e22498b9d4dcd93fda32a2c
出典データセット
uspto-grants-2002_01
特許番号
US06339045B1

反応ノート

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