反应详情

A mixture of 1-(2,5-dihydroxyphenyl)ethanone (3.16 g), benzyl chloride (7.04 g), potassium carbonate (12.4 g) and 18-Crown-6 (30 mg) in 2-butanone (50 ml) was heated under reflux for 5 hrs. After cooling the precipitate was filtered off. The filtrate was evaporated to dryness under reduced pressure and ether (50 ml) was added to it. The solution was washed twice with dilute sodium hydroxide solution, twice with dilute hydrochloric acid, dried over sodium sulphate and substantially evaporated to dryness under reduced pressure. The residue was triturated with cold n-heptane (30 ml), and the precipitate was filtered off with suction filtration giving after drying 2.85 g of 1-[2,5-Bis(benzyloxy)phenyl]ethanone. 1H NMR (400 MHz, DMSO-d6) δ=2.50 (s, 3H), 5.08 (s, 2H), 5.18 (s, 2H), 7.20-7.50 (m, 13H).

1. temperaturewas heated
2. temperatureunder reflux for 5 hrs
3. temperatureAfter cooling the precipitate
4. filtrationwas filtered off
5. customThe filtrate was evaporated to dryness under reduced pressure and ether (50 ml)
6. additionwas added to it
7. washThe solution was washed twice with dilute sodium hydroxide solution, twice with dilute hydrochloric acid
8. dry with materialdried over sodium sulphate
9. customsubstantially evaporated to dryness under reduced pressure
10. customThe residue was triturated with cold n-heptane (30 ml)
11. filtrationthe precipitate was filtered off with suction filtration
12. customgiving
13. dry with materialafter drying 2.85 g of 1-[2,5-Bis(benzyloxy)phenyl]ethanone