Hydrogen chloride-ethyl acetate → Tert-butyl 4-[2-(piperidin-4-yl)ethyl]piperidine-1-carboxylate hydrochloride

HRID 2074281노트

반응식

HRID 2074281 반응식
[ClH:1].CCOC(C)=O.[N:8]1[CH:13]=[CH:12][C:11](/[CH:14]=[CH:15]/[CH:16]2[CH2:21][CH2:20][N:19]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:18][CH2:17]2)=[CH:10][CH:9]=1.[H][H]>[Pt]=O.C(O)C>[ClH:1].[NH:8]1[CH2:9][CH2:10][CH:11]([CH2:14][CH2:15][CH:16]2[CH2:17][CH2:18][N:19]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:20][CH2:21]2)[CH2:12][CH2:13]1

참가 물질

6

반응물 3

HCID 21866389Hydrogen chloride-ethyl acetateHCID 57450068tert-butyl 4-[(E)-2-pyridin-4-ylvinyl]piperidine-1-carboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 57421848Tert-butyl 4-[2-(piperidin-4-yl)ethyl]piperidine-1-carboxylate hydrochloride

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 702Ethanol용매

실험 절차

A 4 M hydrogen chloride/EtOAc solution (0.88 ml) and platinum oxide (100 mg) were added to an ethanol (25 ml) solution of tert-butyl 4-[(E)-2-pyridin-4-ylvinyl]piperidine-1-carboxylate (1.02 g), followed by stirring in the presence of hydrogen (3.5 atm) for 24 hours. This was purged with argon, diluted with methanol, filtered through Celite, and concentrated under reduced pressure. The solid precipitated was washed with EtOAc/hexane, and dried under reduced pressure to obtain tert-butyl 4-(2-piperidin-4-ylethyl)piperidine-1-carboxylate hydrochloride (850 mg) as a white solid.

후처리

  1. customThis was purged with argon
  2. additiondiluted with methanol
  3. filtrationfiltered through Celite
  4. concentrationconcentrated under reduced pressure
  5. customThe solid precipitated
  6. washwas washed with EtOAc/hexane
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-4e3708a7d5aa41fb94098b73366200b2
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07919494B2

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