Sodium Carbonate → 4-(7-Chloro-4-quinolinylamino)-N-[(1-ethyl-2-pyrrolidinyl)-methyl]benzenesulphonamide

HRID 2309373노트

반응식

HRID 2309373 반응식
Cl.[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][CH:15]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.C(=O)([O-])[O-].[Na+].[Na+].[NH2:30][CH2:31][CH:32]1[CH2:36][CH2:35][CH2:34][N:33]1[CH2:37][CH3:38]>C(Cl)(Cl)Cl>[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([S:20]([NH:30][CH2:31][CH:32]4[CH2:36][CH2:35][CH2:34][N:33]4[CH2:37][CH3:38])(=[O:22])=[O:21])=[CH:16][CH:15]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 1172952-Aminomethyl-1-ethylpyrrolidineHCID 201495884-(7-Chloro-4-quinolinylamino)benzenesulphonyl chloride hydrochloride

생성물 1

HCID 137471334-(7-Chloro-4-quinolinylamino)-N-[(1-ethyl-2-pyrrolidinyl)-methyl]benzenesulphonamide수율 39.3%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

4-(7-Chloro-4-quinolinylamino)benzenesulphonyl chloride hydrochloride (23.4 g, 0.06 mol) was added portionwise to a well stirred mixture of aqueous sodium carbonate (60 g in 600 ml water) and 2-aminomethyl-1 ethyl pyrrolidine (7.8 g, 0.06 mol) in chloroform (600 ml) at about 10° C. The ice bath used for cooling was removed and, after 11/2 hours, the mixture was filtered. The chloroform layer was separated and dried (MgSO4). Concentration under reduced pressure caused precipitation of a solid, which was collected by filtration and dried. Recrystallisation from ethanol gave the title compound (10.5 g), melting point 200°-201.5° C.

후처리

  1. temperaturefor cooling
  2. customwas removed
  3. filtrationafter 11/2 hours, the mixture was filtered
  4. customThe chloroform layer was separated
  5. dry with materialdried (MgSO4)
  6. concentrationConcentration under reduced pressure
  7. customprecipitation of a solid, which
  8. filtrationwas collected by filtration
  9. customdried
  10. customRecrystallisation from ethanol

출처 및 근거

ORD 기록
ord-7586fe52ae094a52a17719dbfd088741
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04695574

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