N-(3-Pyridylmethyl)Pyrrolidine → 3-(Pyrrolidin-1-ylmethyl)piperidine

HRID 346517노트

반응식

HRID 346517 반응식
[N:1]1([CH2:6][C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1>C(O)(=O)C.O=[Pt]=O>[N:1]1([CH2:6][CH:7]2[CH2:12][CH2:11][CH2:10][NH:9][CH2:8]2)[CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 1

HCID 67786N-(3-Pyridylmethyl)Pyrrolidine

생성물 1

HCID 43418943-(Pyrrolidin-1-ylmethyl)piperidine

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 176Acetic Acid용매

실험 절차

The educt 3-(1-pyrrolidinylmethyl)-pyridine (24.6 g) is taken up in 250 ml glacial acetic acid and hydrogenated with 2 g of PtO2 under 3 bar H2 at ambient temperature. The solution filtered off is evaporated down, combined with ice and made alkaline with solid KOH while cooling. Afer extracting three times with 250 ml of diethylether the crude product is dried with MgSO4. After the MgSO4 has been filtered off the solvent is eliminated and the amine is distillled in a water jet vacuum at a boiling point of 123° C.

후처리

  1. filtrationThe solution filtered off
  2. customis evaporated down
  3. temperaturewhile cooling
  4. extractionAfer extracting three times with 250 ml of diethylether the crude product
  5. dry with materialis dried with MgSO4
  6. filtrationAfter the MgSO4 has been filtered off the solvent

출처 및 근거

ORD 기록
ord-a02acd3d308042168037de62a9e592d2
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07173028B2

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