Water → HCID 9857126、化合物

HRID 2084358

反応式

HRID 2084358 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11]([NH2:13])=[O:12])=[CH:5][CH:4]=1.[Cl:16][CH2:17][C:18]([CH2:20]Cl)=O.O>C1(C)C=CC=CC=1>[Cl:16][CH2:17][C:18]1[N:13]=[C:11](/[CH:10]=[CH:9]/[C:6]2[CH:5]=[CH:4][C:3]([C:2]([F:14])([F:15])[F:1])=[CH:8][CH:7]=2)[O:12][CH:20]=1

参加物

5

反応物 3

HCID 962WaterHCID 107931,3-DichloroacetoneHCID 57090144-(Trifluoromethyl)cinnamamide

生成物 1

HCID 9857126HCID 9857126、化合物収率 63.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of (E)-3-(4-trifluoromethylphenyl)-2-propenamide (17.9 g) and 1,3-dichloroacetone (14.8 g) in toluene (83 ml) was refluxed under heating for 9 hours using a Dean-Stark apparatus. After cooling, water was added; the reaction mixture was extracted with ethyl acetate and washed with saturated saline, after which it was dried over anhydrous magnesium sulfate. After the solvent was distilled off under reduced pressure, the residue was purified by silica gel column chromatography (eluent: hexane-methyl acetate=6:1→5:1) to yield the titled compound (15.1 g) as a colorless needle crystal.

後処理

  1. temperatureunder heating for 9 hours
  2. temperatureAfter cooling
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. washwashed with saturated saline
  5. dry with materialafter which it was dried over anhydrous magnesium sulfate
  6. distillationAfter the solvent was distilled off under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (eluent: hexane-methyl acetate=6:1→5:1)

出典と根拠

ORDレコード
ord-798c87eca15c434aab6813a671a6242d
出典データセット
uspto-grants-2004_04
特許番号
US06716863B2

関連ノート

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