三氯甲烷 → 5-醛基-2-噻吩甲酸

HRID 268147

反应方程式

HRID 268147 反应方程式
[CH3:1][C:2]1[S:3][C:4]([C:7]([OH:9])=[O:8])=[CH:5][CH:6]=1.C(Cl)(Cl)Cl.BrBr.C(=O)([O-])[O-:17].[Na+].[Na+]>C(Cl)(Cl)(Cl)Cl.[W]>[CH:1]([C:2]1[S:3][C:4]([C:7]([OH:9])=[O:8])=[CH:5][CH:6]=1)=[O:17]

参与物

7

反应物 4

HCID 6212三氯甲烷HCID 10340Carbonic acid sodium salt (1:2)HCID 24408Government regulation2 次HCID 747135-甲基-2-噻吩甲酸

产物 1

HCID 8188825-醛基-2-噻吩甲酸

试剂、催化剂与溶剂 2

HCID 23964钨催化剂HCID 5943四氯化碳溶剂2 次

实验过程

2-Methyl thiophen-5-carboxylic acid was dissolved in carbon tetrachloride (150 ml.) and chloroform (10 ml.) and AZDN (0.5g.) was added. The mixture was refluxed over a 150 watt tungsten spotlight. Two molar equivalents of bromine as a 30% v/v solution in carbon tetrachloride were slowly added. A precipitate was formed but the mixture continued to take up bromine. After the addition of the two molar equivalents, solvent was boiled off until the volume was 100 ml. and the product treated with sodium carbonate solution with gentle heating for two hours to obtain 2-formyl thiophen-5-carboxylic acid in the form of a yellow solid after acidification, extraction and removal of the solvent.

后处理

  1. customA precipitate was formed
  2. additionAfter the addition of the two molar equivalents, solvent
  3. temperaturewith gentle heating for two hours

来源与证据

ORD记录
ord-b6867c0130184750802e3e579b65ce10
来源数据集
uspto-grants-1976_03
专利号
US03947336

关联笔记

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