反应详情

温度

0 °C

A mixture of sodium salt of ethyl 2-hydroxyimino-2-cyanoacetate (16.4 g), water (100 ml) and acetone (15 ml) is stirred at 0°C, and methyl chloroformate (9.4 g) is dropwise added thereto. The resulting mixture is adjusted to pH 7 to 8 with the addition of an aqueous solution of sodium hydrogencarbonate and stirred for 5 hours. The reaction mixture is extracted with ether, and the ether layer is washed with water, dried and concentrated. The residue is recrystallized from a benzene - n-hexane mixture to give ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate (8.4 g) as crystals melting at 69° to 71°C.

1. stirringstirred for 5 hours
2. extractionThe reaction mixture is extracted with ether
3. washthe ether layer is washed with water
4. customdried
5. concentrationconcentrated
6. customThe residue is recrystallized from a benzene - n-hexane mixture