反应详情

A mixture of 11.9 g (45.2 mmol) of N,N-dimethyl-3,5-di-t-butyl-4-hydroxybenzylamine, 18.8 g (37.7 mmol) of di-(1-methoxy-2,2,6,6-tetramethylpiperidin-4-yl) n-butylmalonate, 173 mg of lithium amide, and 100 ml of tetrahydrofuran is refluxed for 90 minutes. The reaction mixture is diluted with ethyl acetate (350 ml). The organic solution is washed with 1N HCl (2×100 ml), water (2×250 ml), and saturated NaHCO3 solution (250 ml), then dried over magnesium sulfate and evaporated to obtain a brown oil. Crystallization from 9:1 methanol:water affords 14.9 g (55% yield) of a white solid (mp 111°-13° C.).

1. temperatureis refluxed for 90 minutes
2. washThe organic solution is washed with 1N HCl (2×100 ml), water (2×250 ml), and saturated NaHCO3 solution (250 ml)
3. dry with materialdried over magnesium sulfate
4. customevaporated
5. customto obtain a brown oil
6. customCrystallization from 9:1 methanol