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Potassium Carbonate → Methyl 4-(4-ethylpiperazin-1-yl)benzoate

HRID 478624
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HRID 478624 반응식
[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7](F)=[CH:6][CH:5]=1.[CH2:12]([N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1)[CH3:13].C(=O)([O-])[O-].[K+].[K+]>CC(N(C)C)=O>[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7]([N:17]2[CH2:18][CH2:19][N:14]([CH2:12][CH3:13])[CH2:15][CH2:16]2)=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 67878Methyl 4-fluorobenzoateHCID 791961-Ethylpiperazine

생성물 1

HCID 57781922Methyl 4-(4-ethylpiperazin-1-yl)benzoate

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

4-Fluorobenzoic acid methyl ester (53 mmol), 1-ethyl-piperazine (44 mmol) and potassium carbonate (44 mmol) are suspended in dimethyl-acetamide (50 ml) and stirred under reflux overnight. After evaporation of the solvent, the residue is dissolved in water and extracted three times with ethyl acetate. The extract is dried over sodium sulfate and evaporated. The residue is suspended in diethylether/pentane and the solid filtered of and dried (vacuum). A brownish powder with mp. 102-104° C., Rf=0.22 (CH2Cl2MeOH=95:5) is obtained.

후처리

  1. temperatureunder reflux overnight
  2. customAfter evaporation of the solvent
  3. dissolutionthe residue is dissolved in water
  4. extractionextracted three times with ethyl acetate
  5. dry with materialThe extract is dried over sodium sulfate
  6. customevaporated
  7. filtrationthe solid filtered of and
  8. customdried (vacuum)
  9. customA brownish powder with mp. 102-104° C., Rf=0.22 (CH2Cl2MeOH=95:5) is obtained

출처 및 근거

ORD 기록
ord-10a2ca4e7f8a42cb85fa11b1a8b11eec
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06642239B2

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