反応式
[OH:1][C@H:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:4][C@H:3]1[C:15]([NH2:17])=O.B.CSC>C1COCC1>[NH2:17][CH2:15][C@H:3]1[C@@H:2]([OH:1])[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:4]1参加物
4
反応条件
- 温度
- 80 °C
実験手順
A solution of (cis)-4-hydroxy-1-(phenylmethyl)-3-piperidinecarboxamide (0.7 g, 3 mmol) in THF (6 ml) was treated with a borane-methyl sulphide complex (2M solution in THF, 3.3 ml). The reaction mixture was heated at 80° C. for 1300 s under microwave irradiation conditions. This was repeated twelve times and then the reaction mixtures were combined and the solvent was removed under reduced pressure and the residue was subjected to column chromatography on silica gel using a dichloromethane, methanol and aqueous ammonia gradient (20% methanol/dichloromethane-20% 2M ammonia in methanol/dichloromethane) to provide 4.6 g of the desired pure compound and 1.1 g of less pure material.
後処理
- customthe reaction mixtures
- customthe solvent was removed under reduced pressure
- customto provide 4.6 g of the desired pure compound and 1.1 g of less pure material
出典と根拠
- ORDレコード
- ord-195aa1c634cc4890bc0ef7b3f3fc6293
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732461B2
関連ノート
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