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Dicyclohexylcarbodiimide → 8-Fluoro-isoquinoline-3-carboxylic acid{(s)-1-azabicyclo[2.2.2]oct-2-yl}-amide

HRID 2245286
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2245286
C1([N:7]=[C:8]=[N:9][CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12]C2)CCCCC1.[F:16][C:17]1[CH:18]=[CH:19][CH:20]=[C:21]2[C:26]=1[CH:25]=[N:24][C:23]([C:27]([OH:29])=O)=[CH:22]2.[CH2:30](N(C(C)C)C(C)C)C.OC1C2N=NNC=2C=CC=1.N12CCC(CC1)[C@H](N)C2>CN(C=O)C>[N:9]12[CH2:10][CH2:15][CH:14]([CH2:13][CH2:12]1)[CH2:30][C@H:8]2[NH:7][C:27]([C:23]1[N:24]=[CH:25][C:26]2[C:21]([CH:22]=1)=[CH:20][CH:19]=[CH:18][C:17]=2[F:16])=[O:29]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 10868DicyclohexylcarbodiimideHCID 81531Diisopropylethylamine2×HCID 719216(S)-quinuclidin-3-amineHCID 685453938-Fluoroisoquinoline-3-carboxylic acidHCID 178418300HCID 178418300, Verbindung

Produkt 1

HCID 68550588
8-Fluoro-isoquinoline-3-carboxylic acid{(s)-1-azabicyclo[2.2.2]oct-2-yl}-amide
Ausbeute 35 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Dicyclohexyl-carbodiimide (7.69 g, 30 mmol) is added to a solution of 8-fluoro-isoquinoline-3-carboxylic acid (5.1 g, 22.4 mmol), ethyl-diisopropyl-amine (4.6 ml, 26.88 mmol) and hydroxybenzotriazole (5.36 g, 33.6 mmol) in DMF (150 ml). The mixture is stirred for 2 hours at room temperature. (S)-(1-Aza-bicyclo[2.2.2]oct-3-yl)amine (4.46 g, 49.28 mmol) and ethyl-diisopropyl-amine (8.7 ml, 49.28 mmol) are added and the solution is stirred for another 18 hours at room temperature. The solvent is removed by evaporation and the residue is dissolved in methylenedichloride and washed with a saturated K2CO3 solution and brine. The organic layer is dried over MgSO4 and evaporated. The crude product is purified by chromatography (CH2Cl2/MeOH/NH4OH, 92.5/7.5/0.75) to afford the desired compound (2.35 g). The product is recrystallized from ethanolic HCl to give 2 g. of the hydrochloric salt.

Aufarbeitung

  1. stirringthe solution is stirred for another 18 hours at room temperature
  2. customThe solvent is removed by evaporation
  3. dissolutionthe residue is dissolved in methylenedichloride
  4. washwashed with a saturated K2CO3 solution and brine
  5. dry with materialThe organic layer is dried over MgSO4
  6. customevaporated
  7. customThe crude product is purified by chromatography (CH2Cl2/MeOH/NH4OH, 92.5/7.5/0.75)

Quellen und Nachweise

ORD-Eintrag
ord-71871602fe904859a754ca0db7e542e5
Quelldatensatz
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07683075B2

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