Dichloromethane → Trichlorothiophene-3-sulfonyl chloride

HRID 1973914

反応式

HRID 1973914 の反応式
[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]

参加物

7

反応物 2

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

生成物 1

HCID 16639974Trichlorothiophene-3-sulfonyl chloride

試薬・触媒・溶媒 4

HCID 6451240Aluminum(III) Chloride触媒HCID 15930840CID 15930840触媒HCID 962Water溶媒HCID 24648Sulfuryl chloride溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-66918658db194bf898b0c2b682c41b23
出典データセット
uspto-grants-1976_12
特許番号
US03998961

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