反应详情

To a solution of sodium β-chloropivalate, prepared from β-chloropivalic acid (13.66 g) and 50% sodium hydride (4.80 g) in dimethylformamide (110 ml) was added dropwise trimethyl chlorosilane (10.85 g) in dimethylformamide (10 ml) at -5° C. to -3° C. After stirring for 1 hour sodium thiobenzoate, prepared from thiobenzoic acid (13.8 g) and 50% sodium hydride (4.80 g) in dimethylformamide (70 ml), was added dropwise thereto at -5° C. to -8° C. After addition of sodium iodide (15.0 g), the mixture was stirred at room temperature for 3 days and then at 40° C. for 7 days. The reaction mixture was diluted with ice-water and extracted with ethyl acetate. The ethyl acetate extract was washed with water, dried over anhydrous sodium sulfate and evaporated in vacuo. The residue was recrystallized from diisopropyl ether-petroleum ether to give β-benzoylthiopivalic acid.

1. additionwas added dropwise
2. customat -5° C. to -8° C
3. waitat 40° C. for 7 days
4. extractionextracted with ethyl acetate
5. extractionThe ethyl acetate extract
6. washwas washed with water
7. dry with materialdried over anhydrous sodium sulfate
8. customevaporated in vacuo
9. customThe residue was recrystallized from diisopropyl ether-petroleum ether