Ethanol → Sodium 1-azabicyclo[3.2.0]heptan-3,7-dione-2-carboxylate

HRID 2198445ノート

反応式

HRID 2198445 の反応式
[N:1]12[C:7](=[O:8])[CH2:6][CH:5]1[CH2:4][C:3](=[O:9])[CH:2]2[C:10]([O:12]CC1C=CC=CC=1)=[O:11].C(O)C.O.C([O-])(O)=O.[Na+:28]>O1CCOCC1.[Pd]>[N:1]12[C:7](=[O:8])[CH2:6][CH:5]1[CH2:4][C:3](=[O:9])[CH:2]2[C:10]([O-:12])=[O:11].[Na+:28]

参加物

7

反応物 4

HCID 702EthanolHCID 962WaterHCID 516892Sodium BicarbonateHCID 12804725Benzyl 3,7-dioxo-1-azabicyclo[3.2.0]heptane-2-carboxylate

生成物 1

HCID 23692747Sodium 1-azabicyclo[3.2.0]heptan-3,7-dione-2-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 312751,4-Dioxane溶媒

実験手順

Benzyl 1-azabicyclo[3.2.0]heptan-3,7-dione-2-carboxylate (25 mg) is hydrogenated at 40 psi for 1 hr in dioxane (2 ml) containing ethanol (0.5 ml), H2O (0.5 ml), NaHCO3 (8.1 mg) and 10% Pd/C (10 mg). The mixture is filtered to remove the catalyst which is washed with more H2O (2.5 ml). The combined filtrate and washing is extracted with EtOAc (3×2 ml), concentrated under reduced pressure, and lyophilized to provide sodium 1-azabicyclo[3.2.0]heptan-3,7-dione-2-carboxylate.

後処理

  1. filtrationThe mixture is filtered
  2. customto remove the catalyst which
  3. washis washed with more H2O (2.5 ml)
  4. washThe combined filtrate and washing
  5. extractionis extracted with EtOAc (3×2 ml)
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e3e0846312c9401ab2f377e447c81629
出典データセット
uspto-grants-1982_11
特許番号
US04357342

反応ノート

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