1-(3-Chlorophenyl)piperazine → 4-(3-Chlorophenyl)-1-(2,3-epoxypropyl)piperazine

HRID 4990

反応式

HRID 4990 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].[CH2:16]([CH:18]1[O:20][CH2:19]1)Cl>>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][N:11]([CH2:16][CH:18]3[O:20][CH2:19]3)[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 13551-(3-Chlorophenyl)piperazineHCID 7835EpichlorohydrinHCID 24758Sodium hydride

生成物 1

HCID 103548864-(3-Chlorophenyl)-1-(2,3-epoxypropyl)piperazine

実験手順

To a mixture of 1.50 g of 4-(3-chlorophenyl)-piperazine and 0.31 g of sodium hydride was added 2.4 ml of epichlorohydrin and the reaction mixture as stirred at room temperature for 30 minutes. After the reaction was completed, the reaction mixture was extracted with 100 ml of ethyl acetate, and the extract was washed 5 times with 100 ml of water, then dried with anhydrous magnesium sulfate. The solvent was removed by evaporation to obtain the residue which was purified by means of a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1) to obtain 1.66 g of 4-(3-chlorophenyl)-1-(2,3-epoxypropyl)piperazine as in the form of an oily substance.

後処理

  1. extractionthe reaction mixture was extracted with 100 ml of ethyl acetate
  2. washthe extract was washed 5 times with 100 ml of water
  3. dry with materialdried with anhydrous magnesium sulfate
  4. customThe solvent was removed by evaporation
  5. customto obtain the residue which
  6. customwas purified by means of a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1)

出典と根拠

ORDレコード
ord-15280f38c7e244d1bfa07303e59094ac
出典データセット
uspto-grants-1993_09
特許番号
US05242919

関連ノート

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