Ammonium formate → 4-(4-Benzyltriazol-2-yl)piperidine

HRID 1068172ノート

反応式

HRID 1068172 の反応式
[CH2:1]([C:8]1[CH:12]=[N:11][N:10]([CH:13]2[CH2:18][CH2:17][N:16](CC3C=CC=CC=3)[CH2:15][CH2:14]2)[N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])=O.[NH4+]>[Pd].CO>[CH2:1]([C:8]1[CH:12]=[N:11][N:10]([CH:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[N:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 211931244-(4-Benzyltriazol-2-yl)-1-benzylpiperidine

生成物 1

HCID 211930964-(4-Benzyltriazol-2-yl)piperidine収率 9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of 4-(4-benzyltriazol-2-yl)-1-benzylpiperidine (627 mg, 1.9 mmol, from Step B), 10% palladium on carbon (400 mg, 0.38 mmol) and ammonium formate (770 mg, 11.3 mmol) in 20 mL MeOH was refluxed for 1 h. The mixture was filtered through celite and concentrated. The residue was dissolved in chloroform and the solution was washed with 1M aqueous NaOH. The organic layer was dried over Na2SO4 and concentrated to afford 41 mg (9%) of product was obtained which was used in the next step without purification.

後処理

  1. temperaturewas refluxed for 1 h
  2. filtrationThe mixture was filtered through celite
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in chloroform
  5. washthe solution was washed with 1M aqueous NaOH
  6. dry with materialThe organic layer was dried over Na2SO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-2d31414e75a44485bee1ef5a92631901
出典データセット
uspto-grants-2001_06
特許番号
US06248755B1

反応ノート

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