5-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]oct-3-ene → 5-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]octane

HRID 249747ノート

反応式

HRID 249747 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]23[CH2:15][N:12]([CH2:13][CH2:14]2)[CH2:11][CH:10]=[CH:9]3)=[CH:4][N:3]=1>[Pt]=O.CO>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]23[CH2:15][N:12]([CH2:13][CH2:14]2)[CH2:11][CH2:10][CH2:9]3)=[CH:4][N:3]=1

参加物

4

反応物 1

HCID 102860575-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]oct-3-ene

生成物 1

HCID 862593785-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]octane収率 71.3%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 887Methanol溶媒

実験手順

1.95 g (7.354 mmol) of 5-(2-bromopyrid-5-yl)-1-azabicyclo[3.2.1]oct-3-ene (WO 03/057 697) are introduced into 40 ml of methanol in a hydrogenation flask, and 195 mg of platinum oxide are then placed in suspension. The medium is stirred at room temperature under a hydrogen pressure of 26 psi for 45 minutes. The reaction medium is filtered through diatomaceous earth and the solvent is removed by evaporation under reduced pressure. The residue obtained is purified by chromatography on a column of silica gel, eluting with a mixture of chloroform, methanol and aqueous ammonia in 95/5/0.5 proportions. 1.4 g of 5-(2-bromopyrid-5-yl)-1-azabicyclo[3.2.1]octane are obtained in the form of a waxy oil.

後処理

  1. filtrationThe reaction medium is filtered through diatomaceous earth
  2. customthe solvent is removed by evaporation under reduced pressure
  3. customThe residue obtained
  4. customis purified by chromatography on a column of silica gel
  5. washeluting with a mixture of chloroform, methanol and aqueous ammonia in 95/5/0.5 proportions

出典と根拠

ORDレコード
ord-ac4081c51618445f8947665f4d47a068
出典データセット
uspto-grants-2011_01
特許番号
US07863290B2

反応ノート

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