反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH:12]=[C:11]([C:14]2[CH:18]=[CH:17][S:16][C:15]=2[C:19]([O:21][CH3:22])=[O:20])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO.[OH-].[OH-].[Pd+2]>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[CH:18]=[CH:17][S:16][C:15]=2[C:19]([O:21][CH3:22])=[O:20])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]参加物
4
実験手順
A solution of 4-(2-methoxycarbonylthiophen-3-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid t-butyl ester (2.5 g, 7.7 mmol, 1.0 eq.) and Pd(OH)2/C (0.5 g, 0.6 mmol) in MeOH (70 mL) was degassed and purged with hydrogen (3×). The mixture was hydrogenated (4 atm) at room temperature overnight, then the vessel was evacuated and purged with nitrogen, and the material was filtered and washed with MeOH (150 mL). The remaining material was concentrated then again was hydrogenated (4 atm) at room temperature overnight. Filtering again as above, and concentrating the filtrate provided 4-(2-methoxycarbonylthiophen-3-yl)piperidine-1-carboxylic acid t-butyl ester (2.4 g).
後処理
- custompurged with hydrogen (3×)
- customat room temperature
- customovernight
- customthe vessel was evacuated
- custompurged with nitrogen
- filtrationthe material was filtered
- washwashed with MeOH (150 mL)
- concentrationThe remaining material was concentrated
- customat room temperature
- customovernight
- filtrationFiltering again as above, and
- concentrationconcentrating the filtrate
出典と根拠
- ORDレコード
- ord-4cf72d806fa54367b63badc338672e7d
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530663B2
関連ノート
読み込み中…