反应详情

To a chilled (0.5° C.) methylene chloride solution of N-cyclobutyl-glycine t-butyl ester (63.2 g, 0.34 mol) and triethylamine (26 g, 0.4 mol) was added dropwise 3-acetylthio-2-methylpropanoyl chloride (61.4 g, 0.34 mol). After stirring overnight the reaction mixture was filtered and the filtrate was concentrated. The residue was redissolved in ethyl acetate, washed with 5% HCl (3×500 ml), brine (500 ml) and saturated aqueous sodium bicarbonate (6×600 ml), dried over MgSO4, filtered, and concentrated yielding 80.6 g (72%) of the product as a brown oil.

1. filtrationwas filtered
2. concentrationthe filtrate was concentrated
3. dissolutionThe residue was redissolved in ethyl acetate
4. washwashed with 5% HCl (3×500 ml), brine (500 ml) and saturated aqueous sodium bicarbonate (6×600 ml)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated