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

HRID 2198445노트

반응식

HRID 2198445 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e3e0846312c9401ab2f377e447c81629
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04357342

반응 노트

불러오는 중…