对羟基苯甲酸 → 3-Methylpentyl p-hydroxybenzoate

HRID 6317

反应方程式

HRID 6317 反应方程式
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.[CH3:11][C@@H:12]([CH2:16][CH3:17])[CH2:13][CH2:14]O.S(=O)(=O)(O)O>C1(C)C=CC=CC=1>[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:14][CH2:13][CH:12]([CH3:11])[CH2:16][CH3:17])=[O:7])=[CH:4][CH:3]=1

参与物

5

反应物 3

HCID 135对羟基苯甲酸HCID 1118四氧化硫HCID 641003(S)-(+)-3-甲基-戊醇

产物 1

HCID 190183233-Methylpentyl p-hydroxybenzoate收率 80.7%

试剂、催化剂与溶剂 1

HCID 1140甲苯溶剂

实验过程

13.7 g of p-hydroxybenzoic acid and 11.4 g of (S)-(+)-3-methyl-1-pentanol were refluxed for 10 hours in toluene in the presence of sulfuric acid, while removing out the generated water from the reaction system. Subsequently, the reaction solution was washed with water to remove the sulfuric acid out. The reaction solution was then dried, concentrated, and purified by column chromatography, to obtain 17.8 g of the objective ester compound (liquid state at room temperature ([α]D23 =+7.8° (CHCl3)). (Yield: 80%)

后处理

  1. customwhile removing out the generated water from the reaction system
  2. washSubsequently, the reaction solution was washed with water
  3. customto remove the sulfuric acid out
  4. customThe reaction solution was then dried
  5. concentrationconcentrated
  6. custompurified by column chromatography

来源与证据

ORD记录
ord-9ad13e2b1c894f9687888c893b7a5b06
来源数据集
uspto-grants-1993_09
专利号
US05248446

关联笔记

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