Chlorosulfonic acid → 4-(2-Sulfamoylethyl)benzenesulfonyl chloride

HRID 1173100ノート

反応式

HRID 1173100 の反応式
[C:1]1([CH2:7][CH2:8][S:9]([NH2:12])(=[O:11])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:13][S:14](O)(=[O:16])=[O:15]>>[S:9]([CH2:8][CH2:7][C:1]1[CH:2]=[CH:3][C:4]([S:14]([Cl:13])(=[O:16])=[O:15])=[CH:5][CH:6]=1)(=[O:10])(=[O:11])[NH2:12]

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 204808Benzeneethanesulfonamide

生成物 1

HCID 223592554-(2-Sulfamoylethyl)benzenesulfonyl chloride収率 77.2%

実験手順

1.3 g (7.3 mmol) of 2-phenylethanesulfonamide was added to 2.4 g (36.5 mmol) of chlorosulfonic acid under ice-cooling over 20 minutes, followed by stirring at room temperature for further 90 minutes. The reaction mixture solution was poured into ice-water, and then extracted with ethyl acetate. The extract was successively washed with an aqueous saturated sodium bicarbonate and brine, and dried over magnesium sulfate. The solvent was evaporated, to give 1.6 g of the title compound.

後処理

  1. temperaturecooling over 20 minutes
  2. extractionextracted with ethyl acetate
  3. washThe extract was successively washed with an aqueous saturated sodium bicarbonate and brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-9ec12645fce04357a1abc45e77bdeb35
出典データセット
uspto-grants-2010_11
特許番号
US07834049B2

反応ノート

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