1,4-Dioxane hydrochloride → 1-{3-[7-(4-Fluoro-phenyl)-imidazo[1,2-a]pyridin-3-yl]-phenyl}-3-(2,2,2-trifluoro-ethyl)-urea hydrochloride salt

HRID 341232

Reaktionsgleichung

Reaktionsgleichung von HRID 341232
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][N:11]3[C:14]([C:17]4[CH:18]=[C:19]([NH:23][C:24]([NH:26][CH2:27][C:28]([F:31])([F:30])[F:29])=[O:25])[CH:20]=[CH:21][CH:22]=4)=[CH:15][N:16]=[C:10]3[CH:9]=2)=[CH:4][CH:3]=1.[ClH:32].O1CCOCC1>CO>[ClH:32].[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][N:11]3[C:14]([C:17]4[CH:18]=[C:19]([NH:23][C:24]([NH:26][CH2:27][C:28]([F:30])([F:29])[F:31])=[O:25])[CH:20]=[CH:21][CH:22]=4)=[CH:15][N:16]=[C:10]3[CH:9]=2)=[CH:4][CH:3]=1

Komponenten

4

Versuchsvorschrift

To a mixture of 1-{3-[7-(4-fluoro-phenyl)-imidazo[1,2-a]pyridin-3-yl]-phenyl}-3-(2,2,2-trifluoro-ethyl)-urea (9.8 g) and methanol (100 mL) was added 4M hydrogen chloride/dioxane (10 mL). The solution was stirred at RT for 90 mins before concentrating under reduced pressure to give the title compound (11.1 g). 1H NMR (400 MHz, DMSO-d6) δ 9.47 (1H, s), 8.81 (1H, d), 8.41 (1H, s), 8.24 (1H, s), 8.03 (3H, dd), 7.95-7.82 (2H, m), 7.60-7.51 (2H, m), 7.50-7.39 (3H, m), 7.37-7.28 (1H, m), 7.14 (1H, t), 4.03-3.42 (7H, m), 3.17 (3H, s).

Aufarbeitung

  1. concentrationbefore concentrating under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f9a64285a1f644a4a7fe6f8f4e5badfa
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08895745B2

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