反应详情

To 40 mL of THF were added 1.8 g (10.8 mmol) of 4-methoxybenzoylhydrazine, 0.9 g (11.5 mmol) of acetyl chloride and 1.1 g of TEA. The reaction mixture was stirred for 1 hour, followed by evaporation off ca. ½ volume of THF. The product was precipitated into methanol, filtered and dried over night under vacuum. Yield was 2.14 g (95%). MS (EI, m/e) calcd for C10H12N2O3 208, found 208 M+, 6.7); mp 146-148° C.

1. customfollowed by evaporation off ca. ½ volume of THF
2. customThe product was precipitated into methanol
3. filtrationfiltered
4. customdried over night under vacuum