2-萘甲醛 → Ethyl 2-methyl-3-beta-naphthyl-acrylate

HRID 1761851笔记

反应方程式

HRID 1761851 反应方程式
[C:1]([CH:8]([CH3:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10])([C:3](OCC)=O)=O.[H-].[Na+].[H][H].[CH:19]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:22]=[CH:21]C=1C=O>C1(C)C(C)=CC=CC=1.O>[CH3:14][C:8](=[CH:1][C:3]1[CH:21]=[CH:22][C:23]2[C:28](=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:19]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参与物

7

反应物 4

HCID 62012-萘甲醛HCID 24758氢化钠HCID 97750草酰丙酸二乙酯HCID 178418361HCID 178418361，化合物

产物 1

HCID 54219653Ethyl 2-methyl-3-beta-naphthyl-acrylate收率 45.2%

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 7237邻二甲苯溶剂2 次

实验过程

40 g (0.2 mol) of ethyl α-ethoxalylpropionate are added to a suspension of 5.5 g (0.2 mol) of 80% strength sodium hydride in 300 ml of absolute xylene at 70° C. When the evolution of hydrogen has ended, 31.2 g (0.2 mol) of β-naphthaldehyde, dissolved in xylene, are added dropwise, and when the addition has ended the mixture is heated at the boiling point for 90 minutes. 150 ml of water are added to the cooled reaction mixture and the organic phase is separated off, washed with 7% strength sodium carbonate solution, dried over sodium sulphate and concentrated. The residue is distilled in vacuo. 21.7 g (45.2% of theory) of ethyl 2-methyl-3-β-naphthyl-acrylate of boiling point 110° C./0.13 mbar are obtained.

后处理

  1. additionare added dropwise
  2. additionwhen the addition
  3. temperatureis heated at the boiling point for 90 minutes
  4. customthe organic phase is separated off
  5. washwashed with 7% strength sodium carbonate solution
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated
  8. distillationThe residue is distilled in vacuo

来源与证据

ORD记录
ord-0c9096043ec04b518637325bc83c8365
来源数据集
uspto-grants-1989_05
专利号
US04829063

反应笔记

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