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

HRID 2050902노트

반응식

HRID 2050902 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b4722c4db17541b5b4e8e699bd51f4bb
출처 데이터셋
uspto-grants-1991_05
특허 번호
US05015656

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