反应详情

To a suspension of 37.4 g (1.00 mole) lithium aluminum hydride in 1000 ml tetrahydrofuran, was added a solution of 88.3 g (0.380 mole) of N-methyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide in tetrafuran dropwise under nitrogen. The reaction was then refluxed overnight. The reaction flask was cooled in an ice bath and 37.4 ml of water, 37.4 ml of 15% sodium hydroxide and and 112.2 ml of water were added. The precipitated solids were filtered and washed with hot ethanol. The combined filtrates were concentrated, then dissolved in dichloromethane, filtered, dried over magnesium sulfate, and the solvent evaporated under reduced pressure to give 68.7 g of N-methyl-1-(phenylmethyl)-3-pyrrolidinemethanamine as an oil. This material was used without further purification in the step.

1. temperatureThe reaction was then refluxed overnight
2. temperatureThe reaction flask was cooled in an ice bath
3. filtrationThe precipitated solids were filtered
4. washwashed with hot ethanol
5. concentrationThe combined filtrates were concentrated
6. dissolutiondissolved in dichloromethane
7. filtrationfiltered
8. dry with materialdried over magnesium sulfate
9. customthe solvent evaporated under reduced pressure