반응 #72733

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5-(2-bromopyrid-5-yl)-1-azabicyclo[3.2.1]oct-3-ene

→

5-(2-bromopyrid-5-yl)-1-azabicyclo[3.2.1]octane

수율 71.3%

용매

methanol

반응 조건

후처리

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

실험 절차

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.

출처