Chloroacetyl chloride → HCID 178514674、化合物

HRID 918187ノート

反応式

HRID 918187 の反応式
[S:1]([C:5]1[CH:11]=[C:10]([S:12](=[O:15])(=[O:14])[NH2:13])[C:9]([Br:16])=[CH:8][C:6]=1[NH2:7])(=[O:4])(=[O:3])[NH2:2].[Cl:17][CH2:18][C:19](Cl)=O>O1CCOCC1>[Cl:17][CH2:18][C:19]1[NH:2][S:1](=[O:3])(=[O:4])[C:5]2[CH:11]=[C:10]([S:12](=[O:14])(=[O:15])[NH2:13])[C:9]([Br:16])=[CH:8][C:6]=2[N:7]=1

参加物

4

反応物 2

HCID 6577Chloroacetyl chlorideHCID 5177804-Amino-6-bromo-1,3-benzenedisulfonamide

生成物 1

HCID 178514674HCID 178514674、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 2,4-disulfamoyl-5-bromoaniline (0.02 mole) and chloroacetyl chloride (0.022 mole) in 75 ml. of dioxane is heated under reflux for about 24 hours and then concentrated to dryness. The residue is dissolved in ethanol and then heated on the steam bath in a mixture of 2.0 g. of potassium or sodium acetate and 50 ml. of water for two hours. The solution is cooled and the product separated by acidification with hydrochloric acid and purified by recrystallization from a mixture of ethanol and water.

後処理

  1. temperatureunder reflux for about 24 hours
  2. concentrationconcentrated to dryness
  3. dissolutionThe residue is dissolved in ethanol
  4. temperatureheated on the steam bath in a mixture of 2.0 g
  5. temperatureThe solution is cooled
  6. customthe product separated by acidification with hydrochloric acid
  7. custompurified by recrystallization from a mixture of ethanol and water

出典と根拠

ORDレコード
ord-29a48bc9dea84cd8804df219eb6e4a9b
出典データセット
uspto-grants-1976_07
特許番号
US03969518

反応ノート

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