Acetic Acid → HCID 70023596, 화합물

HRID 398397노트

반응식

HRID 398397 반응식
C([N:8]1[CH2:12][C@@H:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=2)[C@H:10]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:9]1)C1C=CC=CC=1.C(O)(=O)C>C(O)C.[Pd]>[CH2:22]([O:21][C:19]([C@H:10]1[C@H:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=2)[CH2:12][NH:8][CH2:9]1)=[O:20])[CH3:23]

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 70024099HCID 70024099, 화합물

생성물 1

HCID 70023596HCID 70023596, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A solution of 1-benzyl-trans-3-ethoxycarbonyl-4-(2-pyridyl)pyrrolidine from step 2 above (5.0 g, 16 mmol) and 10% Pd on carbon (750 mg) in ethanol (30 mL) containing acetic acid (3 mL) was shaken under an atmosphere of hydrogen (40 psi) on a Parr apparatus at ambient temperature for 18 h. The catalyst was removed by filtration and the filtrate solvents were removed in vacuo. The residue was partitioned between CH2Cl2 and aqueous NaHCO3. The organic phase was separated, dried over MgSO4, filtered, and concentrated in vacuo to give the title compound as an oil (3.3 g; HPLC RT=2.43 min, method A).

후처리

  1. customThe catalyst was removed by filtration
  2. customthe filtrate solvents were removed in vacuo
  3. customThe residue was partitioned between CH2Cl2 and aqueous NaHCO3
  4. customThe organic phase was separated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-22366045eede442a8928dcbae4c084d6
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610692B1

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