Dichloromethane → 4-Methylphenyl-2-propenal

HRID 478144

반응식

HRID 478144 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]=[O:10])=[CH:4][CH:3]=1.[CH2:11](Cl)Cl.C[N+](C)=C.[I-].[Cl-].[NH4+]>C(N(CC)CC)C>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[CH2:11])[CH:9]=[O:10])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 25517Ammonium ChlorideHCID 61006Lilac acetaldehydeHCID 2724133Dimethyl(methylene)ammounium iodide

생성물 1

HCID 180009044-Methylphenyl-2-propenal

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

2.57 g of aldehyde 37 is introduced into 300 ml of methylene chloride under nitrogen, and 6.5 ml of triethylamine and 7.1 g of Eschenmoser's salt are added at 0° C. After 2.5 hours at 0° C., saturated ammonium chloride solution is added, extracted with methylene chloride, washed with sodium chloride solution, dried on sodium sulfate and concentrated by evaporation. The residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 1.94 g of title compound 38 accumulates as a colorless oil.

후처리

  1. extractionextracted with methylene chloride
  2. washwashed with sodium chloride solution
  3. customdried on sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customThe residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 1.94 g of title compound 38 accumulates as a colorless oil

출처 및 근거

ORD 기록
ord-d8133d68e7694eb5b0601502f575c14f
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06642218B2

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