二氯甲烷 → 4-Methylphenyl-2-propenal

HRID 478144笔记

反应方程式

HRID 478144 反应方程式
[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

参与物

6

反应物 4

HCID 6344二氯甲烷HCID 25517氯化铵HCID 610064-甲基苯乙醛HCID 2724133n,n-二甲基亚甲基碘化胺

产物 1

HCID 180009044-Methylphenyl-2-propenal

试剂、催化剂与溶剂 1

HCID 8471三乙胺溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-d8133d68e7694eb5b0601502f575c14f
来源数据集
uspto-grants-2003_11
专利号
US06642218B2

反应笔记

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