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Sodium Carbonate → 4-(Ethylenedioxy)-1-(diphenylacetyl)piperidine

HRID 1449053
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HRID 1449053 반응식
[C:1]1([CH:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8](Cl)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[Na+].[Na+].[CH2:23]1[CH2:32][O:31][CH:30]2[CH:25]([CH2:26][CH2:27][NH:28][CH2:29]2)[O:24]1>C1C=CC=CC=1>[CH2:23]1[CH2:32][O:31][CH:30]2[CH:25]([CH2:26][CH2:27][N:28]([C:8](=[O:9])[CH:7]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH2:29]2)[O:24]1
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참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 746372,2-Diphenylacetyl chlorideHCID 69545778Octahydro-[1,4]dioxino[2,3-c]pyridine

생성물 1

HCID 705946584-(Ethylenedioxy)-1-(diphenylacetyl)piperidine

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a stirred solution of 24 parts of diphenylacetyl chloride in 250 parts by volume of benzene is added 15 parts of solid sodium carbonate and 16.4 parts of 4-(ethylenedioxy)piperidine. The resultant mixture is refluxed for about 29 hours, left overnight at room temperature, and filtered. The filtrate is washed twice with 10% hydrochloric acid, twice with saturated sodium bicarbonate solution and once with brine. The filtrate is then dried over magnesium sulfate, concentrated and recrystallized from cyclohexane to afford 4-(ethylenedioxy)-1-(diphenylacetyl)piperidine, melting at about 136°-137° C. This compound has the following structural formula ##STR20##

후처리

  1. filtrationfiltered
  2. washThe filtrate is washed twice with 10% hydrochloric acid, twice with saturated sodium bicarbonate solution and once with brine
  3. dry with materialThe filtrate is then dried over magnesium sulfate
  4. concentrationconcentrated
  5. customrecrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-cc7e1189931c4a8b99bd5caf8accbfd3
출처 데이터셋
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04188485

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