反应详情

A mixture of the sodium salt of compound 4 (1.0 g, 3.0 mmol) and chloromethyl acetate (0.4 g, 3.5 mmol) in 18 ml of DMF is stirred at RT for 3 days. The reaction mixture is poured onto ice. The solid which precipitates is collected by filtration, is washed with water and is air-dried. It is stirred in 50 ml of chloroform for 2 hours and is filtered. The filtrate is evaporated to give glass-like material, which is triturated with ether to give the crude product. Purification by prep. TLC gives acetyloxymethyl 2-acetylnicotinate 4-(3-fluorophenyl)semicarbazone, m.p. 159°-160° (compound 54, Table C).

1. additionThe reaction mixture is poured onto ice
2. customThe solid which precipitates
3. filtrationis collected by filtration
4. washis washed with water
5. customis air-dried
6. stirringIt is stirred in 50 ml of chloroform for 2 hours
7. filtrationis filtered
8. customThe filtrate is evaporated
9. customto give glass-like material, which
10. customis triturated with ether
11. customto give the crude product
12. customPurification by prep