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Thionyl Chloride → trans 3-Bromocinnamoyl chloride

HRID 372477
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HRID 372477 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7](O)=[O:8].S(Cl)([Cl:15])=O>C1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7]([Cl:15])=[O:8]
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참가 물질

4

반응물 2

HCID 24386Thionyl Chloride2회HCID 776461m-Bromocinnamic acid

생성물 1

HCID 14959106trans 3-Bromocinnamoyl chloride수율 99.8%

시약·촉매·용매 1

HCID 241Benzene용매2회

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. temperatureto reflux
  2. additionwas added at such a rate as
  3. temperatureto maintain constant reflux
  4. temperatureThe reaction mixture was heated
  5. temperatureat reflux for an additional 2 hr
  6. customThe solvent and excess thionyl chloride were then removed under reduced pressure

출처 및 근거

ORD 기록
ord-1602dc8d2a8c4baa8ab8a88a0ae28d29
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04091112

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