Water → HCID 9857126、化合物

HRID 1610941

反応式

HRID 1610941 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 mixture of (E)-3-(4-trifluoromethylphenyl)-2-propenamide (17.9 g) and 1,3-dichloroacetone (14.8 g) in toluene (83 ml) was refluxed for 9 hours by use of Dean-Stark apparatus. After cooling, the reaction mixture was combined with water, extracted with ethyl acetate, washed with saturated brine, and dried over magnesium sulfate, then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=6:1 to 5:1) to give the titled compound (15.1 g) as colorless needle crystals.

後処理

  1. temperaturewas refluxed for 9 hours by use of Dean-Stark apparatus
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=6:1 to 5:1)

出典と根拠

ORDレコード
ord-f5e6a1b5218143e3a243ec9ba534379d
出典データセット
uspto-grants-2006_01
特許番号
US06984653B2

関連ノート

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