Dichloromethane → 4-Methylphenyl-2-propenal

HRID 478144

反応式

HRID 478144 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 180009044-Methylphenyl-2-propenal

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d8133d68e7694eb5b0601502f575c14f
出典データセット
uspto-grants-2003_11
特許番号
US06642218B2

関連ノート

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