反应详情

Ammonium acetate (240 g, 3114 mmol) was added to a solution of (R)-ethyl 2-methyl-5-oxocyclopentanecarboxylate (106.0 g, 622.8 mmol) in MeOH (1.2 L). The reaction mixture was stirred at room temperature under nitrogen for 20 hours, and the reaction was complete as determined by TLC and HPLC. The reaction mixture was concentrated to remove MeOH. The resulting residue was dissolved in DCM, washed with H2O (2×), brine (1×), dried (Na2SO4), filtered, and concentrated to give (R)-ethyl 2-amino-5-methylcyclopent-1-enecarboxylate (102 g, 97% yield) as an oil. LC/MS (APCI+) m/z 170 [M+H]+.

1. concentrationThe reaction mixture was concentrated
2. customto remove MeOH
3. dissolutionThe resulting residue was dissolved in DCM
4. washwashed with H2O (2×), brine (1×)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated