Water → N-[4-(trifluoromethyl)phenyl]-2-(5-formyl-2-methoxyphenyl)acetamide

HRID 1816570

反応式

HRID 1816570 の反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:20])[CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[O:18][CH3:19])=[CH:5][CH:4]=1.C1N2CN3CN(C2)CN1C3.O.[C:34](=O)(O)[O-:35].[Na+]>FC(F)(F)C(O)=O.C(OCC)(=O)C>[F:1][C:2]([F:21])([F:22])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:20])[CH2:11][C:12]2[CH:17]=[C:16]([CH:34]=[O:35])[CH:15]=[CH:14][C:13]=2[O:18][CH3:19])=[CH:5][CH:4]=1

参加物

7

反応物 4

HCID 962WaterHCID 4101HexamethylenetetramineHCID 516892Sodium BicarbonateHCID 2684094N-[4-(trifluoromethyl)phenyl]-2-(2-methoxyphenyl)acetamide

生成物 1

HCID 22493985N-[4-(trifluoromethyl)phenyl]-2-(5-formyl-2-methoxyphenyl)acetamide

試薬・触媒・溶媒 2

HCID 6422Trifluoroacetic acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1.0 g of N-[4-(trifluoromethyl)phenyl]-2-(2-methoxyphenyl)acetamide was dissolved in 10 mg trifluoroacetic acid, and 0.46 g hexamethylene tetramine was added, and the mixture was reacted at 85° C. for 3 hours. The reaction solution was returned to room temperature, water and ethyl acetate were added, and sodium bicarbonate was further added until the pH reached 8. The reaction solution was extracted with ethyl acetate, washed with brine and dried over anhdydrous magnesium sulfate and the solvent was evaporated. The residue was subjected to silica gel column chromatography, to give 0.7 g of N-[4-(trifluoromethyl)phenyl]-2-(5-formyl-2-methoxyphenyl)acetamide as a colorless oil from fractions eluted with hexane-ethyl acetate (1:1).

後処理

  1. customthe mixture was reacted at 85° C. for 3 hours
  2. customwas returned to room temperature
  3. extractionThe reaction solution was extracted with ethyl acetate
  4. washwashed with brine
  5. dry with materialdried over anhdydrous magnesium sulfate
  6. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-fbf26c4fd6874849ba425fca38a1b74c
出典データセット
uspto-grants-2005_04
特許番号
US06884821B1

関連ノート

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