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].ClN1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[N:20]=[CH:19]C1.[CH:27]([N:30](C(C)C)CC)(C)C>O1CCCC1>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][NH:15][C:27]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[N:20]=[CH:19][N:30]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]参加物
5
実験手順
(S)-2-Aminomethyl-piperidine-1-carboxylic acid tert-butyl ester (1.0 g), 4-chloroquinoxaline (0.768 g) and diisopropylethylamine (0.816 ml) were dissolved in tetrahydrofuran (75 ml) and heated to reflux for 6 hours under an atmosphere of argon. After cooling, the reaction solution was partitioned between ethyl acetate and water. The organic layer was washed with saturated sodium hydrogen carbonate solution, saturated brine, dried and evaporated. The residue was chromatographed over silica gel, eluting with a gradient of 50 to 100% ethyl acetate in hexane. The title compound was obtained as a white foam (1.44 g).
後処理
- temperatureheated
- temperatureto reflux for 6 hours under an atmosphere of argon
- temperatureAfter cooling
- customthe reaction solution was partitioned between ethyl acetate and water
- washThe organic layer was washed with saturated sodium hydrogen carbonate solution, saturated brine
- customdried
- customevaporated
- customThe residue was chromatographed over silica gel
- washeluting with a gradient of 50 to 100% ethyl acetate in hexane
出典と根拠
- ORDレコード
- ord-43773e5d2c34440ca5b5489610e464ec
- 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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