Acetic Acid → HCID 70023596、化合物

HRID 398397ノート

反応式

HRID 398397 の反応式
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]

参加物

5

反応物 2

HCID 176Acetic AcidHCID 70024099HCID 70024099、化合物

生成物 1

HCID 70023596HCID 70023596、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-22366045eede442a8928dcbae4c084d6
出典データセット
uspto-grants-2003_08
特許番号
US06610692B1

反応ノート

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