反应详情

KOH (3.47 g, 61.82 mmol) was added to a solution of (2-Hydroxy-1,1-dimethyl-ethyl)-carbamic acid tert-butyl ester (Preparation 253, 3.9 g, 20.6 mmol) in 1,4-dioxane (30 mL) followed by the slow addition of dimethyl sulphate at room temperature. The mixture was further allowed to stir at room temperature for 48 hours. Reaction mass was filtered through a short pad of celite, washed with DCM (3×50 mL). The combined filtrate was washed with water (2×50 mL), brine (30 mL), dried over sodium sulphate and evaporated in vacuo to afford the title compound as yellow oil in 88% yield, 3.7 g.

1. customReaction mass
2. filtrationwas filtered through a short pad of celite
3. washwashed with DCM (3×50 mL)
4. washThe combined filtrate was washed with water (2×50 mL), brine (30 mL)
5. dry with materialdried over sodium sulphate
6. customevaporated in vacuo