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Tetrahydrofuran → HCID 20288021, 화합물

HRID 126865
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HRID 126865 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9](=[O:19])[CH2:10]P(=O)(OCC)OCC)[CH:6]=[CH:7][CH:8]=1.O1CCCC1.[H-].[Na+].O=[C:28]1[CH2:33][CH2:32][N:31]([C:34]([O:36][CH2:37][CH3:38])=[O:35])[CH2:30][CH2:29]1>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9](=[O:19])[CH2:10][C:28]2[CH2:33][CH2:32][N:31]([C:34]([O:36][CH2:37][CH3:38])=[O:35])[CH2:30][CH:29]=2)[CH:6]=[CH:7][CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 34767Ethyl 4-oxo-1-piperidinecarboxylateHCID 53666596HCID 53666596, 화합물

생성물 1

HCID 20288021HCID 20288021, 화합물수율 83%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
15 °C

실험 절차

To a stirred mixture of 41 parts of diethyl [2-(3-methoxyphenyl)-2-oxoethyl]phosphonate and 180 parts of tetrahydrofuran are added portionwise 5 parts of sodium hydride dispersion 61% while cooling at about 15° C. Upon completion, stirring is continued for 30 minutes at room temperature. Then there are added dropwise 21 parts of ethyl 4-oxo-1-piperidinecarboxylate at about 20° C. Stirring is continued for 4 hours at 60° C. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is distilled, yielding 30 parts (83%) of ethyl 2,3-dihydro-4-[2-(3-methoxyphenyl)-2-oxoethyl]-1(6H)-pyridinecarboxylate; bp. 200°-210° C. at 1 mm. pressure.

후처리

  1. stirringStirring
  2. waitis continued for 4 hours at 60° C
  3. temperatureThe reaction mixture is cooled
  4. customthe layers are separated
  5. customThe organic phase is dried
  6. filtrationfiltered
  7. customevaporated
  8. distillationThe residue is distilled

출처 및 근거

ORD 기록
ord-9a91ce810a6f4335986020b65d21134f
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04254127

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