Water → Trichlorothiophene-3-sulfonyl chloride

HRID 8632

반응식

HRID 8632 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].[S][Cl:13].O>S(Cl)(Cl)(=O)=O.[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

6

반응물 3

HCID 962WaterHCID 27360942,5-Dichlorothiophene-3-sulfonyl chlorideHCID 15930840CID 15930840

생성물 1

HCID 16639974Trichlorothiophene-3-sulfonyl chloride수율 991.6%

시약·촉매·용매 2

HCID 6451240Aluminum(III) Chloride촉매HCID 24648Sulfuryl chloride용매2회

반응 조건

온도
60 °C

실험 절차

A mixture of 2,5-dichlorothiophene-3-sulfonyl chloride (1.2 g, 5 mmol) and sulfur monochloride (10 mg) in sulfuryl chloride (500 mg) was heated at 60° C. for 30 min, at which time was added dropwise a mixture of aluminum trichloride (10 mg) in sulfuryl chloride (500 mg). The reaction was heated at 60° C. for an additional 3 hours, at which time it was allowed to cool to ambient temperature. Cold water (20 mL) was added and the reaction extracted with dichloromethane (2×20 mL). The combined organic layers were washed with saturated sodium bicarbonate solution, dried (Mg2SO4) and concentrated to furnish a tan solid (420 mg, 33%).

후처리

  1. additionwas added dropwise
  2. temperatureThe reaction was heated at 60° C. for an additional 3 hours, at which time it
  3. temperatureto cool to ambient temperature
  4. extractionthe reaction extracted with dichloromethane (2×20 mL)
  5. washThe combined organic layers were washed with saturated sodium bicarbonate solution
  6. dry with materialdried (Mg2SO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2f30ba84e4194cd6b9cb4784c4f11ab7
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091204B2

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