반응 #1252751

반응 방정식

benzylamine

water

potassium hydroxide

water

lithium aluminum hydride

→

1-Benzyl-3-benzylaminopyrrolidine

용매

tetrahydrofuran

tetrahydrofuran

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.WAITThe mixture is left
2. 2
   기타after which 360 g are removed from the resulting solution (3,848 g of total weight)
3. 3
   온도The mixture is refluxed for 20 hours
4. 4
   여과The salts are filtered off with suction
5. 5
   세척washed with tetrahydrofuran
6. 6
   농축the filtrate is concentrated
7. 7
   workup.DISTILLATIONthe residue is distilled

실험 절차

1,000 g (5.34 mols) of 1-benzyl-Δ3 -pyrroline-2,5-dione are dissolved in 2.5 l of tetrahydrofuran, and 572 g (5.34 mols) of benzylamine are added with stirring at 10° to 20° C. The mixture is left to stand for 24 hours at room temperature, after which 360 g are removed from the resulting solution (3,848 g of total weight) and added to a solution of 38 g (1 mol) of lithium aluminum hydride in 380 ml of absolute dehydrated tetrahydrofuran. The mixture is refluxed for 20 hours, 500 ml of tetrahydrofuran, 38 g of water and 120 ml of tetrahydrofuran, 38 g of 10% strength potassium hydroxide solution and 114 g of water are then sucessively added to the mixture. The salts are filtered off with suction, washed with tetrahydrofuran, the filtrate is concentrated, and the residue is distilled.

출처