Water → HCID 9857126, 화합물

HRID 2084358

반응식

HRID 2084358 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 9857126HCID 9857126, 화합물수율 63.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-798c87eca15c434aab6813a671a6242d
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06716863B2

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