反应详情

3-Bromo-5-fluoro-4-hydroxybenzoic acid methyl ester (500 mg, 2.01 mmol; T. Kline et al., J. Med. Chem. 45 (2002), 3112-3129), potassium carbonate (971 mg, 7.03 mmol) and 2-bromoethyl acetate (503 mg, 3.01 mmol) were reacted in DMF (5 ml) at room temperature for 72 h. Then the mixture was partitioned between EA and 2 N hydrochloric acid, and the combined organic extracts were dried over sodium chloride, decanted and evaporated to dryness. The raw material was purified by silica gel chromatography (EA/HEP gradient 0:1 to 4:6) to yield the title compound.

1. customThen the mixture was partitioned between EA and 2 N hydrochloric acid
2. dry with materialthe combined organic extracts were dried over sodium chloride
3. customdecanted
4. customevaporated to dryness
5. customThe raw material was purified by silica gel chromatography (EA/HEP gradient 0:1 to 4:6)