HCID 10634568, compound → HCID 21680573, compound

Participants

Reaction Steps

Compound 15a (7.0 g, 27.7 mmol) was added to 35 g of polyphosphoric ester in 100 mL of methylene chloride and refluxed for 1 h. The reaction mixture was poured onto ice, stirred to hydrolyze the polyphosphoric ester, and the resulting solid was filtered and recrystallized from methanol to give 5.4 g (23.0 mmol, 83% yield) of 16a as white plates: mp 106-108° C. 1H NMR:(ppm) 7.48 (s, 1H), 3.89 (s, 3H), 3.84 (s, 3H), 2.95-2.28 (mult, 5H), 2.22 (s, 3H), 1.18 (d, 3H). Anal. (C14H18O3) C,H.

Provenance & Evidence