Sodium Carbonate → 1-[4-(7-Chloro-4-quinolinylamino)benzenesulphonyl]-4-(4-fluorobenzoyl)piperazine

HRID 568896노트

반응식

HRID 568896 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.Cl.[F:25][C:26]1[CH:39]=[CH:38][C:29]([C:30]([N:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)=[O:31])=[CH:28][CH:27]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)(Cl)Cl.O>[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]([N:35]4[CH2:34][CH2:33][N:32]([C:30](=[O:31])[C:29]5[CH:28]=[CH:27][C:26]([F:25])=[CH:39][CH:38]=5)[CH2:37][CH2:36]4)(=[O:22])=[O:21])=[CH:16][CH:15]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 201495884-(7-Chloro-4-quinolinylamino)benzenesulphonyl chloride hydrochlorideHCID 20149590(4-Fluorophenyl)(piperazin-1-yl)methanone hydrochloride

생성물 1

HCID 136083001-[4-(7-Chloro-4-quinolinylamino)benzenesulphonyl]-4-(4-fluorobenzoyl)piperazine수율 5%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

4-(7-Chloro-4-quinolinylamino)benzenesulphonyl chloride hydrochloride (7.8 g, 0.02 mol) was added portion-wise with stirring to a cold mixture of 1-(4-fluorobenzoyl) piperazine hydrochloride (4.9 g, 0.02 mol) in chloroform (250 ml) and sodium carbonate (24.4 g) in water (250 ml). The cooling bath was removed and the mixture was allowed to warm to room temperature. After 1 hour the chloroform layer was separated and dried (MgSO4). The solvent was removed by evaporation to give a brown gum. Crystallisation from ethanol gave the pure title compound (0.53 g), m.p. 235°-237° C.

후처리

  1. customThe cooling bath was removed
  2. customAfter 1 hour the chloroform layer was separated
  3. dry with materialdried (MgSO4)
  4. customThe solvent was removed by evaporation
  5. customto give a brown gum
  6. customCrystallisation from ethanol

출처 및 근거

ORD 기록
ord-1e8bc2f124ee4488a954bcb07d8efae4
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04730047

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