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Potassium Carbonate → HCID 19077574, 화합물

HRID 485629
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HRID 485629 반응식
[NH:1]1[CH2:11][CH2:10][CH2:9][CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH2:2]1.[Cl:12]C(Cl)(Cl)C(O[CH2:17][C:18]1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=1)=O.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[ClH:12].[CH3:25][O:24][C:21]1[CH:22]=[CH:23][C:18]([CH2:17][N:1]2[CH2:11][CH2:10][CH2:9][CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH2:2]2)=[CH:19][CH:20]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 98969Ethyl nipecotateHCID 13548121(4-Methoxyphenyl)methyl trichloroacetate

생성물 1

HCID 19077574HCID 19077574, 화합물수율 56.4%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To 7 liters of toluene were added 695 grams (4.4M) of ethyl nipecotate, 1304 grams (4.8M) of p-methoxybenzyl trichloroacetate, and 660 grams (4.8M) of potassium carbonate. The mixture was refluxed for 72 hours under a nitrogen atmosphere after which it was cooled, and the solvent was removed in vacuo. The resulting oil was dissolved in chloroform, and the solution was washed with 10% aqueous potassium carbonate followed by 10% aqueous hydrochloric acid. The solution then was dried over sodium sulfate and concentrated in vacuo. The resulting oil was triturated with ethyl ether, yielding 783 grams of the title compound as a solid.

후처리

  1. temperatureThe mixture was refluxed for 72 hours under a nitrogen atmosphere after which it
  2. temperaturewas cooled
  3. customthe solvent was removed in vacuo
  4. dissolutionThe resulting oil was dissolved in chloroform
  5. washthe solution was washed with 10% aqueous potassium carbonate
  6. dry with materialThe solution then was dried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe resulting oil was triturated with ethyl ether

출처 및 근거

ORD 기록
ord-6b52211ab5e141cd8b754a259be45da9
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04537727

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