tert-Butanol → {2-[1-(2-Fluoroethyl)-1H-imidazol-4-yl]-ethyl}-carbamic Acid Tert-Butyl Ester
反応式
[F:1][CH2:2][CH2:3][N+:4]1[CH:12]=[C:11]2[N:6]([C:7](=[O:13])[NH:8][CH2:9][CH2:10]2)[CH:5]=1.CCN(C(C)C)C(C)C.[C:23]([OH:27])([CH3:26])([CH3:25])[CH3:24]>>[C:23]([O:27][C:7](=[O:13])[NH:8][CH2:9][CH2:10][C:11]1[N:6]=[CH:5][N:4]([CH2:3][CH2:2][F:1])[CH:12]=1)([CH3:26])([CH3:25])[CH3:24]参加物
4
実験手順
To a warmed (30° C.) suspension of 2-(2-fluoro-ethyl)-5-oxo-5,6,7,8-tetrahydro-imidazo[1,5-c]pyrimidin-2-ium (1.01 g, 3.82 mmol) in t-butanol (38 ml), was added Hunig's base (1.33 ml, 7.64 mmol) and the mixture heated to reflux under an inert atmosphere for 1.5 h. The mixture was cooled and the solvent evaporated to a yellow semi-solid, which was triterated with dichloromethane. The solid was filtered off and the filtrate purified by silica column chromatography, to yield a colourless solid (0.384 g, 39%).
後処理
- temperatureTo a warmed
- temperaturethe mixture heated
- temperatureto reflux under an inert atmosphere for 1.5 h
- temperatureThe mixture was cooled
- customthe solvent evaporated to a yellow semi-solid, which
- filtrationThe solid was filtered off
- customthe filtrate purified by silica column chromatography
出典と根拠
- ORDレコード
- ord-cf38698c0b614b66b14127fc7c6a06f1
- 出典データセット
- uspto-grants-2010_07
- 特許番号
- US07754746B2
反応ノート
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