反应详情

3-Methyl-butyryl chloride (7.40 mL, 60 mmol) was mixed at 0° C. with Meldrum's acid (2,2-dimethyl-1,3-dioxane-4,6-dione; 8.7 g, 60 mmol), and 4-dimethylaminopyridine (DMAP, 15.1 g, 124 mmol) in DCM. The reaction mixture was allowed to reach r.t. over 1.75 hr. and completion of the reaction was verified by TLC. The reaction mixture was diluted with DCM, was washed 3× with 5% aq. solution of potassium bisulfate and brine. The organic phase was than dried with MgSO4. Crude product 9, 13.36 g) obtained after evaporation was used for next reaction without purification. 1H NMR (500 MHz, CDCl3): δ 1.02 (d, 6H), 1.74 (s, 6H), 2.21 (hp, 1H), 2.99 (d, 2H).

1. washwas washed 3× with 5% aq. solution of potassium bisulfate and brine
2. dry with materialthan dried with MgSO4