反应详情

温度

0 °C

To 50 ml of methanol, cooled to -5°, there is added dropwise 2.62 g (0.022 mol) of thionyl chloride (pot temperature maintained between -5° C. and 0° C.). The solution is stirred at 0° C. for 15 min and to it there is added 7.12 g (0.02 mol) of 1-(4-iodophenyl)-1,4-dihydro-4-oxo-6-methylpyridazine-3-carboxylic acid. (See Example 3). The suspension formed is stirred at room temperature for 3 days and to it there is added 200 ml of water. The suspension that forms is stirred at room temperature for 2 days and is vacuum filtered. The filter cake is air dried to afford 4 g of crude product. The crude product is suspended in 25 ml of chloroform and filtered. The filtrate is concentrated in vacuo to afford 3.5 g (47% yield) of product, mp 185°-187° C.

1. customThe suspension formed
2. stirringis stirred at room temperature for 3 days and to it there
3. stirringThe suspension that forms is stirred at room temperature for 2 days
4. filtrationfiltered
5. customdried
6. customto afford 4 g of crude product
7. filtrationfiltered
8. concentrationThe filtrate is concentrated in vacuo