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Triethylamine → HCID 20144930, Verbindung

HRID 648498
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 648498
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:21])=[O:20])=[CH:17][CH:16]=3)=[CH:9][CH:10]=[N:11]2)=[CH:6][CH:5]=1.Cl.[F:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[S:34]([CH:37]1[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]1)(=[O:36])=[O:35].C(N(CC)CC)C>C(Cl)Cl>[ClH:21].[F:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[S:34]([CH:37]1[CH2:42][CH2:41][N:40]([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)[CH2:39][CH2:38]1)(=[O:35])=[O:36]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 13603946HCID 13603946, VerbindungHCID 13825033HCID 13825033, Verbindung

Produkt 1

HCID 20144930HCID 20144930, VerbindungAusbeute 46,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

(B 5) 4-[[7-(Trifluoromethyl)-4-quinolyl]amino]benzoyl chloride hydrochloride (65.20 g) was added slowly to a stirred mixture of 4-[(2-fluorophenyl)sulfonyl]piperidine hydrochloride (47.0 g) and triethylamine (117.2 ml) in dry methylene chloride (1.01 l) at room temperature. The resultant mixture was stirred at the same temperature for 1 hour and under ice cooling for 0.5 hours. The precipitated powder was collected by filtration, washed with a mixture of methylene chloride and water, and suspended in a mixture of chloroform and methanol. Excess methanolic hydrochloric acid was added to the suspension and the resulting solution was concentrated in vacuo to give an oil. The oil was triturated in a mixture of ethyl acetate and ethanol to give powdery 4-[(2-fluorophenyl)sulfonyl]-1-[4-[[7-(trifluoromethyl)-4-quinolyl]amino]benzoyl]piperidine hydrochloride (46.73 g).

Aufarbeitung

  1. filtrationThe precipitated powder was collected by filtration
  2. washwashed with a mixture of methylene chloride and water
  3. additionsuspended in a mixture of chloroform and methanol
  4. additionExcess methanolic hydrochloric acid was added to the suspension
  5. concentrationthe resulting solution was concentrated in vacuo
  6. customto give an oil
  7. customThe oil was triturated in a mixture of ethyl acetate and ethanol

Quellen und Nachweise

ORD-Eintrag
ord-68169c71ecec4d48bc306bf092c37756
Quelldatensatz
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04735952

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