Sulfuryl chloride → 5-chloro-4-methoxythiophene-3-carboxylic acid

HRID 2050902ノート

反応式

HRID 2050902 の反応式
[CH3:1][O:2][C:3]1[C:4]([C:8]([OH:10])=[O:9])=[CH:5][S:6][CH:7]=1.S(Cl)([Cl:14])(=O)=O>C(Cl)(Cl)Cl>[Cl:14][C:7]1[S:6][CH:5]=[C:4]([C:8]([OH:10])=[O:9])[C:3]=1[O:2][CH3:1]

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 27783794-methoxythiophene-3-carboxylic acid

生成物 1

HCID 27783825-chloro-4-methoxythiophene-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To 4-methoxythiophene-3-carboxylic acid (3.16 g) in chloroform (10 ml) was added freshly distilled sulphuryl chloride (1.8 ml). After the exothermic reaction had subsided the product was extracted into 2N NaOH and washed with chloroform. The aqueous solution was acidified with 2N HCl and extracted into dichloromethane, washed with water, dried over magnesium sulphate and the solvent evaporated. The product was crystallised from dichloromethane/n-hexane.

後処理

  1. customAfter the exothermic reaction
  2. extractionwas extracted into 2N NaOH
  3. washwashed with chloroform
  4. extractionextracted into dichloromethane
  5. washwashed with water
  6. dry with materialdried over magnesium sulphate
  7. customthe solvent evaporated
  8. customThe product was crystallised from dichloromethane/n-hexane

出典と根拠

ORDレコード
ord-b4722c4db17541b5b4e8e699bd51f4bb
出典データセット
uspto-grants-1991_05
特許番号
US05015656

反応ノート

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