Piperazine → 1-(3-Fluoro-1-oxido-2-pyridinyl)piperazine

HRID 1263223노트

반응식

HRID 1263223 반응식
Cl[C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:9].[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>C(O)CCC>[N:10]1([C:2]2[C:7]([F:8])=[CH:6][CH:5]=[CH:4][N+:3]=2[O-:9])[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 49131402-Chloro-3-fluoropyridine N-oxide

생성물 1

HCID 704816081-(3-Fluoro-1-oxido-2-pyridinyl)piperazine

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A solution of 2-chloro-3-fluoropyridine N-oxide (400 mg, 3.0 mmol) and piperazine (1.3 g, 15 mmol) in n-butanol, 15 ml, is stirred at reflux for 20 hours. After concentrating under reduced pressure at 55°-60° C., the residue is chromatographed over silica gel and the crude N-oxide eluted with a 50% methanol-methylene chloride solvent mixture. The appropriate eluate is concentrated to an oily residue of the title compound.

후처리

  1. temperatureat reflux for 20 hours
  2. concentrationAfter concentrating under reduced pressure at 55°-60° C.
  3. customthe residue is chromatographed over silica gel
  4. washthe crude N-oxide eluted with a 50% methanol-methylene chloride solvent mixture
  5. concentrationThe appropriate eluate is concentrated to an oily residue of the title compound

출처 및 근거

ORD 기록
ord-6a3fe72decea4c029480d68a3e741bac
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04456604

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