Dichloromethane → Trichlorothiophene-3-sulfonyl chloride

HRID 1973914

반응식

HRID 1973914 반응식
[Cl:1][C:2]1[S:3][C:4]([Cl:11])=[CH:5][C:6]=1[S:7]([Cl:10])(=[O:9])=[O:8].C(Cl)[Cl:13]>S(Cl)(Cl)(=O)=O.O.[S]Cl.[Cl-].[Cl-].[Cl-].[Al+3]>[Cl:1][C:2]1[S:3][C:4]([Cl:11])=[C:5]([Cl:13])[C:6]=1[S:7]([Cl:10])(=[O:8])=[O:9]

참가 물질

7

반응물 2

HCID 6344DichloromethaneHCID 27360942,5-Dichlorothiophene-3-sulfonyl chloride

생성물 1

HCID 16639974Trichlorothiophene-3-sulfonyl chloride

시약·촉매·용매 4

HCID 6451240Aluminum(III) Chloride촉매HCID 15930840CID 15930840촉매HCID 962Water용매HCID 24648Sulfuryl chloride용매2회

실험 절차

A mixture of 63 g (0.25 mol) 2,5-dichlorothien-3-yl-sulfonyl chloride, 0.5 g sulfur monochloride and 25 g sulfuryl chloride was heated under reflux. To the refluxing reaction was then added dropwise 0.5 g aluminum trichloride in 25 g sulfuryl chloride. The reaction mixture was then heated under reflux for 3 hours, cooled diluted with 400 ml cold water and cooled, with methylene chloride. The methylene chloride extracts were washed with water, saturated aqueous sodium bicarbonate, dried over magnesium sulfate and stripped to give 62 g of 2,4,5-trichlorothien-3-ylsulfonyl chloride, which crystallized from hexane as a solid, m.p. 55° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux
  3. customTo the refluxing reaction
  4. temperatureThe reaction mixture was then heated
  5. temperatureunder reflux for 3 hours
  6. temperaturecooled
  7. washThe methylene chloride extracts were washed with water, saturated aqueous sodium bicarbonate
  8. dry with materialdried over magnesium sulfate

출처 및 근거

ORD 기록
ord-66918658db194bf898b0c2b682c41b23
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03998961

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