Ethanol → Benzoic acid, 3-(aminosulfonyl)-4-chloro-, ethyl ester

HRID 1515411ノート

反応式

HRID 1515411 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[S:11](=[O:14])(=[O:13])[NH2:12].[CH2:15](O)[CH3:16]>>[CH2:15]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([Cl:1])=[C:3]([S:11](=[O:13])(=[O:14])[NH2:12])[CH:4]=1)[CH3:16]

参加物

3

反応物 2

HCID 702EthanolHCID 145684-Chloro-3-sulfamoylbenzoic acid

生成物 1

HCID 15938945Benzoic acid, 3-(aminosulfonyl)-4-chloro-, ethyl ester収率 99%

実験手順

To a suspension of 4-chloro-3-sulfamoyl-benzoic acid (50 g, 212 mmol) in 500 mL ethanol is bubbled HCl gas for 10 minutes. The resulting suspension is then heated at reflux for 16 h, cooled and concentrated in vacuo. The resulting residue is recrystallized from isopronanol to yield 55.9 g (99%) of the title compound as an off-white solid.

後処理

  1. customis bubbled HCl gas for 10 minutes
  2. temperatureThe resulting suspension is then heated
  3. temperatureat reflux for 16 h
  4. temperaturecooled
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue is recrystallized from isopronanol

出典と根拠

ORDレコード
ord-a49ffe99593c4c9c9a5206b847320eb8
出典データセット
uspto-grants-2012_07
特許番号
US08222424B2

反応ノート

読み込み中…