Acetonitrile → [4-(2-Methoxy-ethyl)-piperazin-1-yl]-benzoic acid methyl ester

HRID 478636노트

반응식

HRID 478636 반응식
COC(=O)[C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.Br[CH2:18][CH2:19][O:20][CH3:21].[C:22](=[O:25])([O-])[O-:23].[K+].[K+].[C:28](#N)C>>[CH3:28][O:23][C:22](=[O:25])[C:6]1[CH:5]=[CH:4][CH:9]=[CH:8][C:7]=1[N:10]1[CH2:11][CH2:12][N:13]([CH2:18][CH2:19][O:20][CH3:21])[CH2:14][CH2:15]1

참가 물질

5

반응물 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 15429161Methyl 4-(piperazin-1-yl)benzoate

생성물 1

HCID 69996255[4-(2-Methoxy-ethyl)-piperazin-1-yl]-benzoic acid methyl ester

반응 조건

온도
80 °C

실험 절차

4-(Piperazin-1-yl)-benzoic acid methyl ester (19 mmol), 2-bromoethylmethylether (21 mmol), and potassium carbonate (22.8 mmol) are suspended in acetonitrile (50 ml) and stirred at 80° C. for 8 hours. After evaporation of the solvent, the residue is dissolved in water and extracted three times with CH2Cl2. 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 powder with mp. 103-105° C. is obtained.

후처리

  1. customAfter evaporation of the solvent
  2. dissolutionthe residue is dissolved in water
  3. extractionextracted three times with CH2Cl2
  4. dry with materialThe extract is dried over sodium sulfate
  5. customevaporated
  6. filtrationthe solid filtered of and
  7. customdried (vacuum)
  8. customA powder with mp. 103-105° C. is obtained

출처 및 근거

ORD 기록
ord-1cd1d1cbee6746bc99383690b7f9f84c
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06642239B2

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