反応式
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH:4]([CH3:8])[NH:3]1.[C:9]([O:13][C:14](=[O:24])[NH:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22]Br)[N:17]=1)([CH3:12])([CH3:11])[CH3:10]>CN(C=O)C>[C:9]([O:13][C:14](=[O:24])[NH:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22][N:3]2[CH:4]([CH3:8])[CH2:5][CH2:6][CH2:7][CH:2]2[CH3:1])[N:17]=1)([CH3:12])([CH3:11])[CH3:10]参加物
4
反応条件
- 温度
- 50 °C
実験手順
2,6-Dimethylpiperidine (0.24 mL, 1.74 mmol) was added to a solution of (6-bromomethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (250 mg, 0.87 mmol) in DMF (10 mL) followed by heating at 50° C. and the resulting mixture was stirred for 18 h. The resulting mixture was partitioned between water (10 mL) and CHCl3 (20 mL). The organic layer was washed with H3O, brine, and dried over MgSO4. Concentration in vacuo gave a pale yellow solid. MS m/z: 320.3 (M+H). Calc'd. for C18H29N3O2-319.23.
後処理
- customThe resulting mixture was partitioned between water (10 mL) and CHCl3 (20 mL)
- washThe organic layer was washed with H3O, brine
- dry with materialdried over MgSO4
- concentrationConcentration in vacuo
- customgave a pale yellow solid
出典と根拠
- ORDレコード
- ord-3fc3ef085f324258a1fb269005bd6d96
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07196104B2
関連ノート
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