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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 66731569, 화합물 → HCID 66731652, 화합물

HRID 1963310
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HRID 1963310 반응식
[F:1][C:2]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:3]=1[CH2:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][N:14]=1)[C:8]([O:10][CH3:11])=[O:9]>C(O)(=O)C.[Pt](=O)=O>[F:1][C:2]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:3]=1[CH2:4][CH:5]1[CH2:6][CH:7]([C:8]([O:10][CH3:11])=[O:9])[CH2:12][CH2:13][NH:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 66731569HCID 66731569, 화합물

생성물 1

HCID 66731652HCID 66731652, 화합물수율 96%

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매2회HCID 176Acetic Acid용매

실험 절차

A mixture of methyl 2-(2,5-difluorobenzyl)isonicotinate (6.8 g, 25.83 mmol) and platinum(IV) oxide (0.293 g, 1.29 mmol) in acetic acid (68 mL) was hydrogenated in a Büchi hydrogenator at room temperature and 5 bar for 5 h. More PtO2 (190 mg) was added and the hydrogenation continued at room temperature and 5 bar for additional 80 min. The reaction mixture was filtered through Celite and the catalyst was washed with methanol. The filtrate was concentrated, the residue was dissolved in DCM, washed with satd NaHCO3 and the organic layer was dried using a phase separator. The solvent was evaporated under reduced pressure. The residue was dissolved in iso-hexane/ether and filtered. The solvents were evaporated in vacuo to yield methyl 2-(2,5-difluorobenzyl)piperidine-4-carboxylate (6.65 g, 96%). MS m/z 270 (M+H)+

후처리

  1. customwas hydrogenated in a Büchi hydrogenator at room temperature
  2. customcontinued at room temperature
  3. wait5 bar for additional 80 min
  4. filtrationThe reaction mixture was filtered through Celite
  5. washthe catalyst was washed with methanol
  6. concentrationThe filtrate was concentrated
  7. dissolutionthe residue was dissolved in DCM
  8. washwashed with satd NaHCO3
  9. customthe organic layer was dried
  10. customThe solvent was evaporated under reduced pressure
  11. dissolutionThe residue was dissolved in iso-hexane/ether
  12. filtrationfiltered
  13. customThe solvents were evaporated in vacuo

출처 및 근거

ORD 기록
ord-2ee9df8d87c3420292c356ecde3cd87e
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415378B2

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