Hydrogen Bromide → HCID 18756149、化合物

HRID 433920ノート

反応式

HRID 433920 の反応式
[NH2:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:13])=[CH:7][CH:6]=1)(=[O:4])=[O:3].[BrH:20].BrBr>C(O)(=O)C>[NH2:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([CH:11]([Br:20])[C:12]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[O:13])=[CH:9][CH:10]=1)(=[O:3])=[O:4]

参加物

5

反応物 3

HCID 260Hydrogen BromideHCID 24408BromineHCID 222857924-(2-Oxo-2-phenylethyl)benzene-1-sulfonamide

生成物 1

HCID 18756149HCID 18756149、化合物収率 80%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a mixture of 14.4 g (52 mmol) of 2-(4-aminosulfonylphenyl)-1-phenylethanone in 240 mL of glacial acetic acid stirred under nitrogen, a solution of 24 mL of hydrobromic acid in glacial acetic acid (33%) was added. To the reaction mixture was added slowly 8.4 g (52 mmol) of bromine. It was stirred at room temperature until complete loss of the colour. After concentration, the resulting residue was dissolved in ethyl acetate (500 mL). The organic layer was washed twice with 5% aqueous sodium bicarbonate solution (2×350 mL) and with brine (350 mL). The organic layer was dried, filtered and concentrated in vacuum. The residue was swished in hexane to give 14.9 g (80%) of the desired solid as a white powdered solid.

後処理

  1. stirringIt was stirred at room temperature until complete loss of the colour
  2. concentrationAfter concentration
  3. dissolutionthe resulting residue was dissolved in ethyl acetate (500 mL)
  4. washThe organic layer was washed twice with 5% aqueous sodium bicarbonate solution (2×350 mL) and with brine (350 mL)
  5. customThe organic layer was dried
  6. filtrationfiltered
  7. concentrationconcentrated in vacuum

出典と根拠

ORDレコード
ord-d075e444edbd4641b8a3e85e9a16c4fb
出典データセット
uspto-grants-2003_12
特許番号
US06670365B1

反応ノート

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