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Isopropylamine → 3-Bromo-N-isopropylcinnamamide

HRID 372478
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HRID 372478 반응식
BrC1C=C(C=CC=1)/C=C/C(Cl)=O.C(N)(C)C.[Br:17][C:18]1[CH:19]=[C:20]([CH:29]=[CH:30][CH:31]=1)/[CH:21]=[CH:22]/[C:23]([NH:25][CH:26]([CH3:28])[CH3:27])=[O:24]>C1(C)C=CC=CC=1.CCOCC>[Br:17][C:18]1[CH:19]=[C:20]([CH:29]=[CH:30][CH:31]=1)[CH:21]=[CH:22][C:23]([NH:25][CH:26]([CH3:28])[CH3:27])=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6363IsopropylamineHCID 14959106trans 3-Bromocinnamoyl chlorideHCID 20327747trans 3-bromo-N-isopropylcinnamamide

생성물 1

HCID 543874693-Bromo-N-isopropylcinnamamide

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

실험 절차

Trans m-bromocinnamic acid (11.4 g) in dry benzene (75 ml) was heated to reflux and then a mixture of thionyl chloride (12 g) in dry benzene (50 ml) was added at such a rate as to maintain constant reflux. The reaction mixture was heated at reflux for an additional 2 hr after the addition of thionyl chloride. The solvent and excess thionyl chloride were then removed under reduced pressure to give trans 3-bromocinnamoyl chloride (ca. 12.3 g). A solution of the 3-bromocinnamoyl chloride in toluene (150 ml) was added dropwise with stirring to a solution of isopropylamine (10 g) in ether (200 ml). The reaction mixture was stirred at room temperature for one hour and then heated at reflux for one hour. The solvent and excess amine were removed under reduced pressure. The crude residue was triturated with water, filtered, and recrystallized from ethanol-water to give white, crystalline trans 3-bromo-N-isopropylcinnamamide, m.p. 85°-86° C. Elemental analysis, NMR and IR spectra all confirmed the identity of the product.

후처리

  1. temperatureheated
  2. temperatureat reflux for one hour
  3. customThe solvent and excess amine were removed under reduced pressure
  4. customThe crude residue was triturated with water
  5. filtrationfiltered
  6. customrecrystallized from ethanol-water
  7. customto give white

출처 및 근거

ORD 기록
ord-69b158fab0494eae97533fb39f3a3773
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04091112

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