反应详情

温度

0 °C

To a solution of di(4-nitrophenyl) 2-(4-methylbenzyl)succinate (2.4 g) in N,N-dimethylformamide (30 ml) was added a solution of cis-3a,4,7,7a-tetrahydroisoindoline (0.62 g) in N,N-dimethylformamide (10 ml) with stirring at 0° C. After stirring at 0° C. for 3 hours, water was added to the reaction mixture and extracted with ethyl acetate. The organic layer was washed successively with three 1N sodium hydroxide solutions, 1N-hydrochloric acid, and brine and dried over MgSO4. After the solvent was evaporated under reduced pressure, the residue was recrystallized from hexane-ethyl acetate (4:1) to give 1.7 g of 4-nitrophenyl 2-(4-methylbenzyl)-3-(cis-3a,4,7,7a-tetrahydro-2-isoindolinylcarbonyl)propionate.

1. stirringAfter stirring at 0° C. for 3 hours
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed successively with three 1N sodium hydroxide solutions, 1N-hydrochloric acid, and brine
4. dry with materialdried over MgSO4
5. customAfter the solvent was evaporated under reduced pressure
6. customthe residue was recrystallized from hexane-ethyl acetate (4:1)