Potassium Carbonate → 2-(3-Methylpyridin-4-yl)-7-[5-(trifluoromethyl)pyridin-2-yl]-2,7-diazaspiro[4.5]decan-1-one

HRID 1044368

Reaktionsgleichung

[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:19][CH2:18][CH2:17][C:11]3([C:15](=[O:16])[NH:14][CH2:13][CH2:12]3)[CH2:10]2)=[N:7][CH:8]=1.O1CCOCC1.CN[C@H]1[CH2:35][CH2:34][CH2:33][CH2:32][C@@H:31]1[NH:36][CH3:37].BrC1C=CN=CC=1C.C(=O)([O-])[O-].[K+].[K+]>[Cu]I>[CH3:35][C:34]1[CH:37]=[N:36][CH:31]=[CH:32][C:33]=1[N:14]1[CH2:13][CH2:12][C:11]2([CH2:17][CH2:18][CH2:19][N:9]([C:6]3[CH:5]=[CH:4][C:3]([C:2]([F:1])([F:20])[F:21])=[CH:8][N:7]=3)[CH2:10]2)[C:15]1=[O:16]

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

To a solution of 7-[5-(trifluoromethyl)pyridin-2-yl]-2,7-diazaspiro[4.5]decan-1-one (24.4 mg, 0.0000814 mol) in 1,4-dioxane (0.5 mL, 0.006 mol) were added (1S,2S)-N,N′-dimethylcyclohexane-1,2-diamine (2.3 mg, 0.000016 mol), copper(I) iodide (1.6 mg, 0.0000081 mol), 4-bromo-3-methylpyridine (28 mg, 0.00016 mol) and potassium carbonate (23.6 mg, 0.000171 mol); and the mixture was stirred at 100° C. overnight. The product was purified by prep-HPLC. LC-MS: 391.2 (M+H)+.

Aufarbeitung

customThe product was purified by prep-HPLC

Quellen und Nachweise

ORD-Eintrag: ord-6b60341a343343a29aa4cfb05807c313
Quelldatensatz: uspto-grants-2013_10
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08563570B2

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