Sodium ethoxide → Ethyl 1-Ethyl-2,4-dioxopiperidine-3-carboxylate

HRID 1252279노트

반응식

HRID 1252279 반응식
[Na].[O-]CC.[Na+].[CH2:6]([O:8][C:9]([CH2:11][C:12]([N:14]([CH2:22][CH3:23])[CH2:15][CH2:16][C:17]([O:19]CC)=O)=[O:13])=[O:10])[CH3:7]>C(O)C>[C:9]([CH:11]1[C:17](=[O:19])[CH2:16][CH2:15][N:14]([CH2:22][CH3:23])[C:12]1=[O:13])([O:8][CH2:6][CH3:7])=[O:10]

참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 13784117ethyl N-ethoxycarbonylacetyl-3-ethylaminopropionate

생성물 1

HCID 13784118Ethyl 1-Ethyl-2,4-dioxopiperidine-3-carboxylate수율 71%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

5.8 g of metallic sodium was added to 300 ml of ethanol and they were reacted to obtain an ethanol solution containing sodium ethoxide. To this solution was added 62.2 g of ethyl N-ethoxycarbonylacetyl-3-ethylaminopropionate, and they were refluxed for 4 hours and allowed to cool. Ethanol was distilled off. Thereto were added ethyl acetate and a dilute aqueous hydrochloric acid solution and the resulting mixture was shaken. The organic layer was separated, water-washed, dried and concentrated to obtain 36.3 g of 3-carboethoxy-1-ethylpiperidine-2,4-dione as an oily matter with an yield of 71%.

후처리

  1. customwere reacted
  2. temperaturewere refluxed for 4 hours
  3. temperatureto cool
  4. distillationEthanol was distilled off
  5. additionThereto were added ethyl acetate
  6. customThe organic layer was separated
  7. washwater-washed
  8. customdried
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1fd6fe2772494ec993726d59493f8be5
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04742165

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