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

HRID 478636ノート

反応式

HRID 478636 の反応式
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

参加物

5

反応物 4

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

生成物 1

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

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1cd1d1cbee6746bc99383690b7f9f84c
出典データセット
uspto-grants-2003_11
特許番号
US06642239B2

反応ノート

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