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

HRID 461172노트

반응식

HRID 461172 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
30 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9238b6692c214bc99dc8d0a44ec7240c
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061761

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