Chloroform → Methyl 3-(2-piperidinyl)propanoate hydrochloride

反応式

[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[O:10].C(Cl)(Cl)[Cl:14]>C1COCC1.O=[Pt]=O>[ClH:14].[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[CH2:7][CH2:8][C:9]([O:11][CH3:12])=[O:10]

参加物

実験手順

Methyl 3-(pyridin-2-yl)acrylate (22.15 g, 136 mmol) was dissolved in THF (300 ml) and chloroform (10.9 ml), and PtO2 (3.08 g, 13.6 mmol, 0.1 eq.) was added under a nitrogen atmosphere. The solution was first rinsed with nitrogen for 10 min and was then stirred overnight under a H2 atmosphere (8 bar). After cooling, rinsing with nitrogen was first carried out again, the catalyst was removed by filtering over filtering earth and then rinsed with DCM, and the filtrate was concentrated to dryness in vacuo. The methyl 3-(piperidin-2-yl)propionate hydrochloride was used in the next stage without being purified further.