反应详情

A solution of 20.4 g (0.14 mol) of 3,3-dimethyl-1-methylthio-2-butanone, 19.6 g (0.28 mol) of hydroxylamine hydrochloride and 14.8 g (0.14 mol) of anhydrous sodium carbonate in 140 ml of 95 percent ethanol and 80 ml of water was heated at reflux for 16 hrs. The resulting nearly colorless solution was stripped of volatiles on a rotary evaporator to yield a two layered liquid residue. This residue was extracted with four portions of ethyl acetate. The organic extract was dried over magnesium sulfate, filtered from the drying agent and stripped of solvent. Distillation of the residue gave the desired product as a colorless liquid, b. 83° C./0.6 mm Hg, nD22 1.4989.

1. temperatureat reflux for 16 hrs
2. customThe resulting nearly colorless solution was stripped of volatiles on a rotary evaporator
3. customto yield a two layered liquid residue
4. extractionThis residue was extracted with four portions of ethyl acetate
5. extractionThe organic extract
6. dry with materialwas dried over magnesium sulfate
7. filtrationfiltered from the drying agent
8. distillationDistillation of the residue