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

HRID 1645239

반응식

HRID 1645239 반응식
[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]

참가 물질

5

반응물 2

HCID 6212ChloroformHCID 53733726Methyl 3-(2-pyridyl)-2-propenoate

생성물 1

HCID 47000747Methyl 3-(2-piperidinyl)propanoate hydrochloride

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  1. washThe solution was first rinsed with nitrogen for 10 min
  2. temperatureAfter cooling
  3. washrinsing with nitrogen
  4. customthe catalyst was removed
  5. filtrationby filtering
  6. filtrationover filtering earth
  7. washrinsed with DCM
  8. concentrationthe filtrate was concentrated to dryness in vacuo
  9. customwithout being purified further

출처 및 근거

ORD 기록
ord-71c88d92b1124036883e326911ef9ce3
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124624B2

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