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Dichloromethane → HCID 86742082, Verbindung

HRID 648506
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 648506
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]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 13603946HCID 13603946, VerbindungHCID 13825050HCID 13825050, Verbindung

Produkt 1

HCID 86742082HCID 86742082, Verbindung

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-c67dc822dd1943519f0bae8251ebd547
Quelldatensatz
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04735952

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