Reaktionsgleichung
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]1[N:12]=[CH:11][C:10]2[CH:13]=[N:14][N:15]([C:16]3[N:21]=[C:20]([N:22]4[CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][CH2:23]4)[CH:19]=[CH:18][CH:17]=3)[C:9]=2[CH:8]=1>Cl.O1CCOCC1>[N:22]1([C:20]2[N:21]=[C:16]([N:15]3[C:9]4[CH:8]=[C:7]([C:2]5[CH:3]=[N:4][CH:5]=[CH:6][N:1]=5)[N:12]=[CH:11][C:10]=4[CH:13]=[N:14]3)[CH:17]=[CH:18][CH:19]=2)[CH2:23][CH2:24][NH:25][CH2:26][CH2:27]1Komponenten
4
Versuchsvorschrift
To a solution of tert-butyl 4-[6-(6-pyrazin-2-ylpyrazolo[4,3-c]pyridin-1-yl)-2-pyridyl]piperazine-1-carboxylate (30 mg, 0.065 mmol) in hydrogen chloride (4 mol/l) in 1,4-dioxane (1.5 ml, 6.0 mmol) and 1,4-dioxane; 1.5 mL was stirred at RT 18 h. The reaction was concentrated and submitted for reverse phase HPLC to give 144 (12 mg) in 34% yield. MS (ESI) m/z: 359.1. 1H NMR (400 MHz, DMSO) δ 9.70 (s, 1H), 9.65 (d, J=1.1 Hz, 1H), 9.34 (s, 1H), 8.78-8.74 (m, 1H), 8.72 (d, J=2.4 Hz, 1H), 8.68 (d, J=5.3 Hz, 1H), 7.77 (t, J=8.1 Hz, 1H), 7.25 (d, J=7.7 Hz, 1H), 6.79 (d, J=8.4 Hz, 1H), 3.67-3.61 (m, 4H), 2.97-2.90 (m, 4H).
Aufarbeitung
- concentrationThe reaction was concentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-14d2aafa9a2a4891b9010ce13d9699c3
- Quelldatensatz
- uspto-grants-2016_09
- Patentnummer
- US09434725B2
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