反应详情

温度

60 °C

A mixture of 2′-hydroxy-5′-methylacetophenone (1.0 g, 6.7 mmol) was treated with paraformaldehyde (0.18 g) and conc. hydrochloric acid (5 ml) and the mixture heated at 60° C. overnight. Upon cooling the mixture was extracted with toluene (3×30 ml) and the combined extracts were dried (Na2SO4) and the solvent removed to yield a yellow oil. The oil was treated with methanol (30 ml) and heated to reflux for 1 h. Upon cooling, the solution was evaporated to near dryness, and the residue chromatographed on a silica column, eluting with 0-10% ethyl acetate in petroleum ether. The purified product was obtained as an white powder (0.76 g)

1. temperatureUpon cooling the mixture
2. extractionwas extracted with toluene (3×30 ml)
3. dry with materialthe combined extracts were dried (Na2SO4)
4. customthe solvent removed
5. customto yield a yellow oil
6. temperatureheated
7. temperatureto reflux for 1 h
8. temperatureUpon cooling
9. customthe solution was evaporated
10. customthe residue chromatographed on a silica column
11. washeluting with 0-10% ethyl acetate in petroleum ether