Tert-Butylamine → 3-(Tert-butylsulfamoyl)-4-chlorobenzoic acid

HRID 461172ノート

反応式

HRID 461172 の反応式
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[Cl:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][C:8]=1[S:16](Cl)(=[O:18])=[O:17]>C(O)C>[C:1]([NH:5][S:16]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][C:7]=1[Cl:6])[C:11]([OH:13])=[O:12])(=[O:17])=[O:18])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 6385Tert-ButylamineHCID 756134-Chloro-3-(chlorosulphonyl)benzoic acid

生成物 1

HCID 23938783-(Tert-butylsulfamoyl)-4-chlorobenzoic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
30 °C

実験手順

To a mixture of 36.5 g (0.5 mol) of tert.-butylamine and 250 ml of ethanol were added 25.5 g (0.1 mol) of 4-chloro-3-chlorosulfonylbenzoic acid in small portions while stirring and cooling, the reaction temperature being maintained at about 30° C. After a dwelling time over night at room temperature, the solvent was distilled off, the residue was dissolved in about 200 ml of water, the pH was adjusted to 1 with concentrated HCl and the crystals were filtered off. Melting point: 250° C.

後処理

  1. temperaturecooling
  2. waitAfter a dwelling time over night at room temperature
  3. distillationthe solvent was distilled off
  4. dissolutionthe residue was dissolved in about 200 ml of water
  5. filtrationthe crystals were filtered off

出典と根拠

ORDレコード
ord-9238b6692c214bc99dc8d0a44ec7240c
出典データセット
uspto-grants-1977_12
特許番号
US04061761

反応ノート

読み込み中…