反应详情

温度

150 °C

6-(2-Methoxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran (3.5 g) (see Preparation 7) was dissolved in dry 2,4,6-collidine (15 ml), anhydrous lithium iodide (9.0 g) was added and the mixture was heated at 150° C. for 40 hours. After cooling, the mixture was taken up in dichloromethane and washed with 2N aqueous hydrochloric acid solution (×3). The organic layer was dried (anhydrous sodium sulphate), the solvent removed under reduced pressure and the residue was chromatographed on silica using 1:1 hexane: dichloromethane as the eluent to yield 6-(2-hydroxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran (1.2 g) as an oil.

1. temperatureAfter cooling
2. washwashed with 2N aqueous hydrochloric acid solution (×3)
3. dry with materialThe organic layer was dried (anhydrous sodium sulphate)
4. customthe solvent removed under reduced pressure
5. customthe residue was chromatographed on silica using 1:1 hexane