反応 #549682

反応方程式

hydrogen bromide

sulphur trioxide

4-(3-methyl-2-pyridyl)butylamine dihydrobromide

→

4-(5-bromo-3-methyl-2-pyridyl)-butylamine

収率 51.5%

溶媒

dichloromethane

1,1,2-trifluorotrichloroethane

1,1,2-trifluorotrichloroethane

反応条件

後処理

1. 1
   その他prepared
2. 2
   温度the mixture was heated
3. 3
   温度under reflux for ca 16 hr
4. 4
   その他The solvent was removed by distillation
5. 5
   その他was removed by acetylation

実験手順

A solution of sulphur trioxide (150 ml) in 1,1,2-trifluorotrichloroethane (350 ml) was added over ca 30 min. to a suspension of 4-(3-methyl-2-pyridyl)butylamine dihydrobromide (17 g) [prepared by passing hydrogen bromide gas through a solution of the amine in dichloromethane] in 1,1,2-trifluorotrichloroethane (100 ml) and the mixture was heated under reflux for ca 16 hr. The solvent was removed by distillation and unbrominated starting material was removed by acetylation as described in Example 1(b) to yield 4-(5-bromo-3-methyl-2-pyridyl)-butylamine (6.53 g) as an oil.

出典