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Dichloromethane → HCID 86742082, 화합물

HRID 648506
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HRID 648506 반응식
Cl.[F:2][C:3]([F:25])([F:24])[C:4]1[CH:13]=[C:12]2[C:7]([C:8]([NH:14][C:15]3[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=3)=[CH:9][CH:10]=[N:11]2)=[CH:6][CH:5]=1.Cl.[N:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[S:33](C1CCNCC1)=[O:34].C([N:43]([CH2:46][CH3:47])[CH2:44][CH3:45])C.[CH2:48](Cl)Cl>>[N:43]1[CH:44]=[CH:45][CH:48]=[CH:47][C:46]=1[CH:29]1[CH2:30][CH2:31][CH2:32][N:27]([C:19](=[O:20])[C:18]2[CH:22]=[CH:23][C:15]([NH:14][C:8]3[C:7]4[C:12](=[CH:13][C:4]([C:3]([F:25])([F:24])[F:2])=[CH:5][CH:6]=4)[N:11]=[CH:10][CH:9]=3)=[CH:16][CH:17]=2)[C:28]1=[S:33]=[O:34]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 13603946HCID 13603946, 화합물HCID 13825050HCID 13825050, 화합물

생성물 1

HCID 86742082HCID 86742082, 화합물

실험 절차

4-[[7-(Trifluoromethyl)-4-quinolyl]amino]benzoyl chloride hydrochloride (0.69 g) was added slowly to a stirred mixture of 4-[(2-pyridyl)sulfinyl]piperidine hydrochloride (0.50 g) and triethylamine (1.72 ml) in dry methylene chloride (22 ml) at room temperature. The resultant mixture was stirred at the same temperature for 1.5 hours and concentrated in vacuo. The residue was partitioned between chloroform and water. The organic layer was washed with saturated aqueous sodium bicarbonate, dried over magnesium sulfate, and concentrated to dryness in vacuo. The resultant crystalline residue was recrystallized from a mixture of methylene chloride and methanol and washed successively with methanol and methylene chloride to give 4-[(2-pyridyl(sulfinyl]-1-[4-[[7-(trifluoromethyl)-4-quinolyl]amino]benzoyl]piperidine (0.59 g).

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue was partitioned between chloroform and water
  3. washThe organic layer was washed with saturated aqueous sodium bicarbonate
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated to dryness in vacuo
  6. customThe resultant crystalline residue was recrystallized from a mixture of methylene chloride and methanol
  7. washwashed successively with methanol and methylene chloride

출처 및 근거

ORD 기록
ord-c67dc822dd1943519f0bae8251ebd547
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04735952

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