Sodium Carbonate → 1-[4-Fluorobenzoyl]-4-[4-(7-trifluoromethyl-4-quinolinylamino)benzenesulphonyl]piperazine

HRID 1788697노트

반응식

HRID 1788697 반응식
Cl.[F:2][C:3]([F:26])([F:25])[C:4]1[CH:13]=[C:12]2[C:7]([C:8]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([S:21](Cl)(=[O:23])=[O:22])=[CH:17][CH:16]=3)=[CH:9][CH:10]=[N:11]2)=[CH:6][CH:5]=1.Cl.[F:28][C:29]1[CH:42]=[CH:41][C:32]([C:33]([N:35]2[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]2)=[O:34])=[CH:31][CH:30]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)(Cl)Cl.O>[F:28][C:29]1[CH:42]=[CH:41][C:32]([C:33]([N:35]2[CH2:40][CH2:39][N:38]([S:21]([C:18]3[CH:19]=[CH:20][C:15]([NH:14][C:8]4[C:7]5[C:12](=[CH:13][C:4]([C:3]([F:26])([F:25])[F:2])=[CH:5][CH:6]=5)[N:11]=[CH:10][CH:9]=4)=[CH:16][CH:17]=3)(=[O:23])=[O:22])[CH2:37][CH2:36]2)=[O:34])=[CH:31][CH:30]=1

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 201495894-(7-Trifluoromethyl-4-quinolinylamino)benzenesulphonyl chloride hydrochlorideHCID 20149590(4-Fluorophenyl)(piperazin-1-yl)methanone hydrochloride

생성물 1

HCID 136082991-[4-Fluorobenzoyl]-4-[4-(7-trifluoromethyl-4-quinolinylamino)benzenesulphonyl]piperazine수율 20.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

4-(7-Trifluoromethyl-4-quinolinylamino)benzenesulphonyl chloride hydrochloride (3.5 g, 0.008 mol) was added portionwise to a cold (10°), well stirred mixture of 1-(4-fluorobenzoyl)piperazine hydrochloride (2.0 g, 0.008 mol) in chloroform (50 ml) and sodium carbonate (10.0 g) in water (50 ml). The cooling bath was removed and the mixture was allowed to warm to room temperature. After half an hour, the mixture was filtered and the filtrate separated. The chloroform layer was dried (MgSO4). The solvent was removed by evaporation to give a yellow gum. The gum was crystallised from ethanol-water, then purified by column chromatography (basic Al2O3-chloroform) followed by recrystallisation from ethanol, to give the pure title compound (0.9 g), m.p. 172°-174.5° C.

후처리

  1. customThe cooling bath was removed
  2. waitAfter half an hour
  3. filtrationthe mixture was filtered
  4. customthe filtrate separated
  5. dry with materialThe chloroform layer was dried (MgSO4)
  6. customThe solvent was removed by evaporation
  7. customto give a yellow gum
  8. customThe gum was crystallised from ethanol-water
  9. custompurified by column chromatography (basic Al2O3-chloroform)
  10. customfollowed by recrystallisation from ethanol

출처 및 근거

ORD 기록
ord-b2a1885435394c86a9ae7fb2a5c46883
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04684657

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