反应详情

2.6 g of 2-[p-(4-methoxy phenyl)-phenyl]-1,3-dioxolane, 0.917 g of hydroxylamine hydrochloride, 40 ml of 1.8 M hydrochloric ethanol and 10 ml of ethanol are introduced into a 100 ml three-necked flask under nitrogen. The reaction mixture is heated to reflux for 4 hours then concentrated under vacuum. The residue is taken up in 30 ml of water, then 220 ml of methyl ter-butyl ether (MTBE) is added. The organic phase is separated and the aqueous phase is extracted with MTBE (2×20 ml). The organic phases are combined, washed with a saturated solution of sodium chloride, dried over anhydrous magnesium sulphate and concentrated under vacuum (yield: 75%).

1. temperatureThe reaction mixture is heated
2. temperatureto reflux for 4 hours
3. concentrationthen concentrated under vacuum
4. addition220 ml of methyl ter-butyl ether (MTBE) is added
5. customThe organic phase is separated
6. extractionthe aqueous phase is extracted with MTBE (2×20 ml)
7. washwashed with a saturated solution of sodium chloride
8. dry with materialdried over anhydrous magnesium sulphate
9. concentrationconcentrated under vacuum (yield: 75%)