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Sulfuric Acid → Ethyl 3-ethoxy-4-oxo-1-piperidinecarboxylate

HRID 345554
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반응식

HRID 345554 반응식
[CH2:1]([O:3][CH:4]1[C:9](OC)([O:10]C)[CH2:8][CH2:7][N:6]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:5]1)[CH3:2].S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O>[CH2:1]([O:3][CH:4]1[C:9](=[O:10])[CH2:8][CH2:7][N:6]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:5]1)[CH3:2]
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참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 15096762HCID 15096762, 화합물

생성물 1

HCID 15096763Ethyl 3-ethoxy-4-oxo-1-piperidinecarboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 34.1 parts of ethyl 3-ethoxy-4,4-dimethoxy-1-piperidinecarboxylate and 1110 parts of a sulfuric acid solution 1% in water was stirred and refluxed for 3 hours. The reaction mixture was cooled and saturated with sodium carbonate. The product was extracted with dichloromethane. The extract was washed with a small amount of water, dried, filtered and evaporated. The residue was stirred in petroleumether. The product was separated and distilled, yielding 21.1 parts of ethyl 3-ethoxy-4-oxo-1-piperidinecarboxylate bp. ±95° C. at 0.05 mm. pressure (intermediate 68).

후처리

  1. temperaturerefluxed for 3 hours
  2. extractionThe product was extracted with dichloromethane
  3. washThe extract was washed with a small amount of water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. stirringThe residue was stirred in petroleumether
  8. customThe product was separated
  9. distillationdistilled

출처 및 근거

ORD 기록
ord-9d754a29280e41aa8e24d98ba561ce75
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05057525

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