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Methanol → 2-Piperidineacetic acid ethyl ester hydrochloride

HRID 1881678
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HRID 1881678 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].C(Cl)(Cl)[Cl:14].CO>C(O)C.O=[Pt]=O>[ClH:14].[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9]
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참가 물질

6

반응물 3

HCID 887MethanolHCID 6212Chloroform2회HCID 75960Ethyl 2-pyridylacetate

생성물 1

HCID 242012202-Piperidineacetic acid ethyl ester hydrochloride

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 702Ethanol용매

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온도
40 °C

실험 절차

Ethyl 2-(pyridin-2-yl)acetate (24.51 g, 148.4 mmol) was dissolved in ethanol (130 ml), and PtO2 (3.37 g, 14.84 mmol, 0.1 eq.) and chloroform (20 ml) were added. The suspension was stirred under an H2 atmosphere (8 bar) at 40° C. overnight. According to TLC control (silica gel, MC/methanol 95:5), the reaction was not complete, so that further chloroform (15 ml) was added and the mixture was stirred under an H2 atmosphere (8 bar) at 40° C. for a further 2 d (TLC control). After cooling, the catalyst was first removed by filtering over filtering earth and the filtrate was concentrated to dryness in vacuo. The ethyl 2-(piperidin-2-yl)acetate hydrochloride was employed in the next stage without further purification.

후처리

  1. stirringthe mixture was stirred under an H2 atmosphere (8 bar) at 40° C. for a further 2 d (TLC control)
  2. temperatureAfter cooling
  3. customthe catalyst was first removed
  4. filtrationby filtering
  5. filtrationover filtering earth
  6. concentrationthe filtrate was concentrated to dryness in vacuo
  7. customThe ethyl 2-(piperidin-2-yl)acetate hydrochloride was employed in the next stage without further purification

출처 및 근거

ORD 기록
ord-7701260652c740b399edc0f3d0b34a14
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318769B2

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