HCID 20255250, 화합물 → 1-(2-Methoxyphenyl)-1-oxo-1lambda~5~-piperazine

HRID 463722노트

반응식

HRID 463722 반응식
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

참가 물질

3

반응물 1

HCID 20255250HCID 20255250, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-242bc0218b494e81bd459c7c1e6cdc85
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04544657

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