反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C@H:9]1[CH2:14][NH2:15])=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl[C:17]1[C:26]([CH3:27])=[N:25][C:24]2[C:19](=[CH:20][C:21]([F:29])=[C:22]([F:28])[CH:23]=2)[N:18]=1>CN(C=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C@H:9]1[CH2:14][NH:15][C:17]1[C:26]([CH3:27])=[N:25][C:24]2[C:19](=[CH:20][C:21]([F:29])=[C:22]([F:28])[CH:23]=2)[N:18]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]参加物
4
反応条件
- 温度
- 90 °C
実験手順
(S)-2-Aminomethyl-piperidine-1-carboxylic acid tert-butyl ester (1.14 g), and 2-chloro-6,7-difluoro-3-methylquinoxaline Teng et al PCT Int. Appl (2000), WO00/42026A1 20000720 (1.14 g) were dissolved in DMF (2 ml) and heated to 90° C. for 3 days under an atmosphere of argon. After cooling, the reaction solution was partitioned between ethyl acetate and water. The organic layer was washed with water, saturated brine, dried and evaporated. The residue was chromatographed over silica gel, eluting with a gradient of 10 to 50% ethyl acetate in hexane. The title compound was obtained as a pink foam (0.524 g), MH+ 393.
後処理
- temperatureAfter cooling
- customthe reaction solution was partitioned between ethyl acetate and water
- washThe organic layer was washed with water, saturated brine
- customdried
- customevaporated
- customThe residue was chromatographed over silica gel
- washeluting with a gradient of 10 to 50% ethyl acetate in hexane
出典と根拠
- ORDレコード
- ord-e387087c8a394279bd035d0d571cc60a
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741329B2
関連ノート
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