反応 #69920

反応方程式

4-(2-methoxycarbonylthiophen-3-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid t-butyl ester

→

4-(2-methoxycarbonylthiophen-3-yl)piperidine-1-carboxylic acid t-butyl ester

収率 95.8%

溶媒

MeOH

反応条件

後処理

1. 1
   その他purged with hydrogen (3×)
2. 2
   その他at room temperature
3. 3
   その他overnight
4. 4
   その他the vessel was evacuated
5. 5
   その他purged with nitrogen
6. 6
   ろ過the material was filtered
7. 7
   洗浄washed with MeOH (150 mL)
8. 8
   濃縮The remaining material was concentrated
9. 9
   その他at room temperature
10. 10
    その他overnight
11. 11
    ろ過Filtering again as above, and
12. 12
    濃縮concentrating the filtrate

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).

出典