反应详情

12.8 g of 2-methoxymethyloxy-4,5,6-trimethoxybenzaldehyde prepared in Referential Example 11 was dissolved in 100 ml of dichloromethane, and 8.7 g of m-chloroperbenzoic acid was added thereto at room temperature while stirring. The mixture was refluxed for 30 min and cooled with ice, and 100 ml of a saturated aqueous sodium thiosulfate solution was added thereto. The precipitated crystals were separated by filtration. The mother liquor was washed with a saturated aqueous sodium hydrogen-carbonate solution, dried over anhydrous magnesium sulfate and concentrated. The residue was mixed with 50 ml of ethanol, 40 ml of water and 21.3 g of potassium hydroxide, and the mixture was stirred for 1 hr under reflux. The reaction mixture was cooled, poured into dilute hydrochloric acid and extracted with ethyl acetate. The organic phase was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off to prepare 11.5 g of the product compound (light yellow oleaginous) as a crude product.

1. temperatureThe mixture was refluxed for 30 min
2. additionwas added
3. customThe precipitated crystals were separated by filtration
4. washThe mother liquor was washed with a saturated aqueous sodium hydrogen-carbonate solution
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. additionThe residue was mixed with 50 ml of ethanol, 40 ml of water and 21.3 g of potassium hydroxide
8. stirringthe mixture was stirred for 1 hr
9. temperatureunder reflux
10. temperatureThe reaction mixture was cooled
11. additionpoured into dilute hydrochloric acid
12. extractionextracted with ethyl acetate
13. washThe organic phase was washed with water
14. dry with materialdried over anhydrous magnesium sulfate
15. distillationthe solvent was distilled off
16. customto prepare 11.5 g of the product compound (light yellow oleaginous) as a crude product