Methanol → 2-[4-(4-氯-1-丁酰基)苯基]-2-甲基丙酸甲酯

HRID 411908笔记

反应方程式

HRID 411908 反应方程式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([OH:16])=[O:15])=[CH:9][CH:8]=1)=[O:6].[CH3:19]O>Cl>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([O:16][CH3:19])=[O:15])=[CH:9][CH:8]=1)=[O:6]

参与物

4

反应物 2

HCID 887MethanolHCID 109235674-[4-氯-1-丁酰基]-A,A-二甲基苯乙酸

产物 1

HCID 100623382-[4-(4-氯-1-丁酰基)苯基]-2-甲基丙酸甲酯收率 95.1%

试剂、催化剂与溶剂 1

HCID 313盐酸溶剂2 次

实验过程

Dissolve 2-[4-(4-chloro-butyryl)-phenyl]-2-methyl-propionic acid (6.2 g, 23.1 mmol) in hot methanolic solution of anhydrous hydrogen chloride (42 mL of a methanol containing 3.2 g of anhydrous hydrogen chloride). Reflux for 42 minutes, evaporate the solvent in vacuo, dissolve the residue in methylene chloride and wash with water. Dry (MgSO4), filter through silica gel, washing the gel with methylene chloride. Combine the organic washings and evaporate the solvent in vacuo to give the title compound as a clear oil (6.21 g, 94%).

后处理

  1. temperatureReflux for 42 minutes
  2. customevaporate the solvent in vacuo
  3. dissolutiondissolve the residue in methylene chloride
  4. washwash with water
  5. dry with materialDry (MgSO4)
  6. filtrationfilter through silica gel
  7. washwashing the gel with methylene chloride
  8. customevaporate the solvent in vacuo

来源与证据

ORD记录
ord-0bfff4e7d8b442118e776fed1afb5023
来源数据集
uspto-grants-2003_05
专利号
US06559312B2

反应笔记

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