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Methanol → methyl (2R,4S)-4-hydroxypiperidine-2-carboxylate

HRID 2185436
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2185436
C1([C@@H]([N:9]2[CH2:15][CH2:14][C@@H:13]3[CH2:16][C@H:10]2[C:11](=[O:17])[O:12]3)C)C=CC=CC=1.[CH3:18][OH:19]>[Pd]>[CH3:18][O:19][C:11](=[O:17])[C@H:10]1[CH2:16][C@@H:13]([OH:12])[CH2:14][CH2:15][NH:9]1
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Komponenten

4

Edukt 2

HCID 887MethanolHCID 10823407(1S,5R)-2-[(1S)-1-phenylethyl]-6-oxa-2-azabicyclo[3.2.1]octan-7-one

Produkt 1

HCID 11321108methyl (2R,4S)-4-hydroxypiperidine-2-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23938PalladiumKatalysator

Versuchsvorschrift

A mixture of (1S,5R)-2-((S)-1-phenylethyl)-6-oxa-2-azabicyclo[3.2.1]octan-7-one (2.95 g) and 10% palladium on activated carbon (570 mg) in methanol (75 mL) was stirred at room temperature for 6 hr under hydrogen (3.5 kgf/cm2). The catalysts were removed by filtration and washed with methanol. The combined organic layers were evaporated in vacuo. A mixture of the residue and 10% palladium on activated carbon (500 mg) in methanol (75 mL) was stirred at room temperature for 8 hr under hydrogen (3.5 kgf/cm2). The catalysts were removed by filtration and washed with methanol. The combined organic layers were evaporated in vacuo. The mixture of the residue and 10% palladium on activated carbon (504 mg) in methanol (75 mL) was stirred at room temperature for 8 hr under hydrogen (4.0 kgf/cm2). The catalysts were removed by filtration and washed with methanol. The combined organic layers were evaporated in vacuo to give the title compound (2.11 g): 1H NMR (400 MHz, CDCl3) δ 1.32-1.49 (m, 2H), 1.83 (br s, 2H), 1.93-1.95 (m, 1H), 2.27-2.32 (m, 1H), 2.61-2.69 (m, 1H), 3.22 (dt, J=12.7, 3.9 Hz, 1H), 3.39 (dd, J=2.9, 10.7 Hz, 1H), 3.71-3.78 (m, 1H), and 3.75 (m, 3H).

Aufarbeitung

  1. customThe catalysts were removed by filtration
  2. washwashed with methanol
  3. customThe combined organic layers were evaporated in vacuo
  4. additionA mixture of the residue and 10% palladium on activated carbon (500 mg) in methanol (75 mL)
  5. stirringwas stirred at room temperature for 8 hr under hydrogen (3.5 kgf/cm2)
  6. customThe catalysts were removed by filtration
  7. washwashed with methanol
  8. customThe combined organic layers were evaporated in vacuo
  9. additionThe mixture of the residue and 10% palladium on activated carbon (504 mg) in methanol (75 mL)
  10. stirringwas stirred at room temperature for 8 hr under hydrogen (4.0 kgf/cm2)
  11. customThe catalysts were removed by filtration
  12. washwashed with methanol
  13. customThe combined organic layers were evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2b74b0b6790a48f9a8be37f807a46715
Quelldatensatz
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06399629B1

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