Acetic Anhydride → HCID 117635545, compound

Participants

Reaction Steps

In a 10 dram vial, added 1-7 (300 mg, 0.795 mmol) to pyridine (3975 μl) followed by acetic anhydride (225 μl, 2.385 mmol) and DMAP (9.71 mg, 0.080 mmol). After 1 h, LCMS showed complete consumption of R1 desired product. Partitioned between 10 mL H2O and 10 mL EtOAc, separated layers. Back-extracted aqueous with 1×5 mL EtOAc. Washed combined organics with 5×5 mL H2O. Dried combined organics over Na2SO4, filtered, concentrated to give a pale yellow oil. Purification by normal-phase HPLC (40 g ISCO column, 0-50% EtOAc:Hexanes) gave 7-1 as a clear, colorless oil.

Provenance & Evidence