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

HRID 2074281ノート

反応式

HRID 2074281 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4e3708a7d5aa41fb94098b73366200b2
出典データセット
uspto-grants-2011_04
特許番号
US07919494B2

反応ノート

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