4-(2,5-Difiuorobenzyl)pyridine → 4-[(2,5-Difluorophenyl)methyl]piperidine

HRID 273734ノート

反応式

HRID 273734 の反応式
[F:1][C:2]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:3]=1[CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1>C(O)(=O)C.[Pt]=O>[F:1][C:2]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:3]=1[CH2:4][CH:5]1[CH2:6][CH2:7][NH:8][CH2:9][CH2:10]1

参加物

4

反応物 1

HCID 200942684-(2,5-Difiuorobenzyl)pyridine

生成物 1

HCID 233550784-[(2,5-Difluorophenyl)methyl]piperidine収率 72.9%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 176Acetic Acid溶媒

実験手順

A mixture of platinum oxide (0.5 g) and 4-(2,5-difluorobenzyl)pyridine from above in acetic acid (100 ml) was hydrogenated for 3 hr. The catalyst was removed and the solution concentrated in vacuo. The residue was dissolved in water and the solution basified with sodium hydroxide. The basic mixture was extracted with ether and the extracts concentrated in vacuo. The crude oil was vacuum distilled to give the product (5.1 g, 72.9%, bp: 110° C.). A sample of the hydrochloride was prepared in ether (mp: 182°-183° C.). Calc'd. for C12H15F2N.HCl: C, 58.19%; H, 6.52%; N, 5.66%. Found: C, 58.14%; H, 6.56%; N, 5.59%.

後処理

  1. customThe catalyst was removed
  2. concentrationthe solution concentrated in vacuo
  3. dissolutionThe residue was dissolved in water
  4. extractionThe basic mixture was extracted with ether
  5. concentrationthe extracts concentrated in vacuo
  6. distillationdistilled

出典と根拠

ORDレコード
ord-3e59270ad6cb427cbe872ae0bed39c5c
出典データセット
uspto-grants-1995_02
特許番号
US05387593

反応ノート

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