3-Methylthiophene → 3-Methylthiophene-2-sulfonyl chloride

HRID 1730067

반응식

HRID 1730067 반응식
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][CH:3]=1.[Cl:7][S:8](O)(=[O:10])=[O:9]>C(Cl)(Cl)Cl.C(=O)(O)[O-].[Na+]>[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[S:8]([Cl:7])(=[O:10])=[O:9]

참가 물질

5

반응물 2

HCID 120243-MethylthiopheneHCID 24638Chlorosulfonic acid

생성물 1

HCID 134257133-Methylthiophene-2-sulfonyl chloride

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 516892Sodium Bicarbonate용매

반응 조건

온도
25 °C

실험 절차

A 49-g (0.5 mol) sample of 3-methylthiophene was added in small portions to a cooled solution (-20° C) of 128 g (1 mol) chlorosulfonic acid in 250 cc chloroform. After the addition was completed, the reaction mixture was allowed to warm to about 25° C and then heated at reflux for 30 minutes. The reaction mixture was then diluted with ice water and neutralized with aqueous sodium bicarbonate solution. The organic layer was separated, dried over magnesium sulfate and evaporated to give 30 g of 3-methyl-2-thienylsulfonyl chloride.

후처리

  1. additionAfter the addition
  2. temperatureheated
  3. temperatureat reflux for 30 minutes
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

출처 및 근거

ORD 기록
ord-daee733669fe41d397471f0f084a84c8
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03991081

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