反应详情

1e was heated at 80° C. in the presence of MeOH (2.5 mL and 1N NaOH 0.5 mL) for 40 min. LC-MS showed completion of the reaction. The solvent was concentrated, and 1N HCl was added followed by the addition of Et2O. The Et2O layer was separated and was washed with H2O (2×), brine, dried over MgSO4, filtered, and concentrated to dryness. The resulting crude if was used directly in the next step: LC-MS (ESI) 312.1 (M+H) (10-90% MeOH in H2O with 0.1% TFA in a 4 min run, tR=3.51 min).

1. customcompletion of the reaction
2. concentrationThe solvent was concentrated
3. addition1N HCl was added
4. additionfollowed by the addition of Et2O
5. customThe Et2O layer was separated
6. washwas washed with H2O (2×), brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated to dryness