反应详情

A solution of the compound obtained in Step A (500 mg) and O-methylhydroxylamine hydrochloride (165 mg) in 15 ml of pyridine is heated at reflux for 3 hours. The reaction mixture is hydrolysed using 100 ml of ice-cold water, acidified using 6N HCl and then extracted with ethyl acetate. The organic phase is dried over magnesium sulphate and evaporated to dryness under reduced pressure. The residue is then purified on silica gel, eluant AcOEt/PE 2/8, to yield the title compound in the form of a white oil (wax).

1. temperatureat reflux for 3 hours
2. extractionextracted with ethyl acetate
3. dry with materialThe organic phase is dried over magnesium sulphate
4. customevaporated to dryness under reduced pressure
5. customThe residue is then purified on silica gel, eluant AcOEt/PE 2/8