反应详情

A solution of the product from Step B above (730 mg) in 10 mL of dichloromethane was cooled to 0° C. and treated dropwise with 5 mL of trifluoroacetic acid. The solution was warmed to room temperature and, after 1 h, concentrated under reduced pressure. The residue was dissolved in methanol and applied to an ion-exchange column (Varian Bond-Elut SCX, 5 g; preconditioned with methanol). The column was washed several times with methanol, and the amine product was eluted with 1.0M ammonia-methanol. The fractions containing product were concentrated under reduced pressure to afford the title compound as an orange oil. LC/MS 136.1 (M+1).

1. concentrationconcentrated under reduced pressure
2. dissolutionThe residue was dissolved in methanol
3. washThe column was washed several times with methanol
4. washthe amine product was eluted with 1.0M ammonia-methanol
5. additionThe fractions containing product
6. concentrationwere concentrated under reduced pressure