反応 #64956

反応方程式

methyl iodide

trans-1-benzyl-3-benzylmethylamino-4-hydroxy-pyrrolidine

sodium hydride

hydrogen

→

trans-1-Benzyl-3-benzylmethylamino-4-methoxypyrrolidine

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度the mixture is heated
2. 2
   温度under reflux at the same time
3. 3
   温度the mixture is then heated
4. 4
   温度under reflux overnight
5. 5
   抽出extracted with toluene
6. 6
   乾燥the extracts are dried with K2CO3
7. 7
   濃縮concentrated
8. 8
   workup.DISTILLATIONthe residue is distilled

実験手順

17.3 g (58 mmol) of crude trans-1-benzyl-3-benzylmethylamino-4-hydroxy-pyrrolidine in 80 ml of absolute tetrahydrofuran are added dropwise to 2.8 g (93.3 mmol) of 80% strength sodium hydride in 40 ml of absolute tetrahydrofuran and the mixture is heated under reflux at the same time. When the evolution of hydrogen has ended, 8.7 g (61 mmol) of methyl iodide are added dropwise and the mixture is then heated under reflux overnight. It is poured into ice-water and extracted with toluene, the extracts are dried with K2CO3 and concentrated and the residue is distilled.

出典