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

HRID 2185436
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HRID 2185436 반응식
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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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2b74b0b6790a48f9a8be37f807a46715
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06399629B1

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