HCID 20255250、化合物 → 1-(2-Methoxyphenyl)-1-oxo-1lambda~5~-piperazine

HRID 463722ノート

反応式

HRID 463722 の反応式
C([CH:5]1[CH2:10][N+:9]([O-:19])([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])[CH2:8][CH2:7][N:6]1C([O-])=O)(C)(C)C>FC(F)(F)C(O)=O>[CH3:18][O:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[N+:9]1([O-:19])[CH2:8][CH2:7][NH:6][CH2:5][CH2:10]1

参加物

3

反応物 1

HCID 20255250HCID 20255250、化合物

生成物 1

HCID 135605501-(2-Methoxyphenyl)-1-oxo-1lambda~5~-piperazine収率 74.4%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

To a stirred ice cold solution of 260 ml trifluoroacetic acid there was added under nitrogen, 26 g of tert-butyl-4-(2-methoxyphenyl)-1-piperazinecarboxylate 4-oxide and stirred for another 6 hours at ambient temperature. The solvent was removed in vacuo. The slurry was taken up in 200 ml ether and extracted twice with each 150 ml of water. The aqueous solution was applied to a column packed with 500 g Dowex 2 (×4, 20-50 mesh, OH- form) and the N-oxide-base eluted with water. After evaporation of the solvent in vacuo, the white foam (18.6 g) was dissolved in a minumum of methylene chloride and the base precipitated by addition of diisopropylether to give 13.1 g colorless hygroscopic crystals of 1-(2-methoxyphenyl)piperazine 1-oxide, mp 157°-160°. The dihydrochloride was crystallized from ethanol/ether, mp 192°-194°.

後処理

  1. customThe solvent was removed in vacuo
  2. extractionextracted twice with each 150 ml of water
  3. washthe N-oxide-base eluted with water
  4. customAfter evaporation of the solvent in vacuo
  5. dissolutionthe white foam (18.6 g) was dissolved in a minumum of methylene chloride
  6. customthe base precipitated by addition of diisopropylether

出典と根拠

ORDレコード
ord-242bc0218b494e81bd459c7c1e6cdc85
出典データセット
uspto-grants-1985_10
特許番号
US04544657

反応ノート

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