反应详情

温度

160 °C

cis-2-Benzyl-6-cyclopropyl-3a-methyl-2,3,3a,4,5,9b-hexahydro-1H-benzo[e]isoindole (0.359 mmol, 75 mg) was dissolved in toluene (1 ml). ACE-Cl (1.654 mmol, 182 μl) was added and the reaction mixture; was heated in a microwave reactor at 160° C. for 15 minutes. MeOH (1 ml) was added and the mixture was again heated in a microwave reactor at 160° C. for 5 minutes. The resulting mixture was passed through an SCX cartridge and the resulting filtrate was concentrated in vacuo to give a crude residue that was purified by preparative-HPLC. To the pure fractions was added HCl in ether (1 ml) and the resulting solution was concentrated in vacuo to afford cis-6-cyclopropyl-3a-methyl-2,3,3a,4,5,9b-hexahydro-1H-benzo[e]isoindole hydrochloride (8.8 mg), m/z: 228.2 [M+H]+.

1. temperaturethe mixture was again heated in a microwave reactor at 160° C. for 5 minutes
2. concentrationthe resulting filtrate was concentrated in vacuo
3. customto give a crude residue that
4. customwas purified by preparative-HPLC
5. additionTo the pure fractions was added HCl in ether (1 ml)
6. concentrationthe resulting solution was concentrated in vacuo