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

HRID 1263223ノート

反応式

HRID 1263223 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6a3fe72decea4c029480d68a3e741bac
出典データセット
uspto-grants-1984_06
特許番号
US04456604

反応ノート

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