反应详情

温度

5 °C

To a 500 ml, 4-necked flask fitted with a stirrer, thermometer, addition funnel and reflux condenser is charged sulfuric acid (50 ml) and methyl m-fluorobenzoate (8.5 g, 0.055 mole). The reaction mixture is then cooled to 5° C. and a solution of potassium nitrate (reagent 5.57 g, 0.055 mole) is concentrated sulfuric acid (50 ml) is added dropwise over a 30 minute period. Ten minutes after completion of addition the reaction mixture is poured onto 500 g of cracked ice and the product extracted into benzene (3×100 ml). The combined benzene extracts are dried with anhydrous magnesium sulfate and the filtrate reduced in vacuo to give 10.6 g (96%) of product, which is a yellow liquid. Anal. Calcd. for C8H6FNO4 : C, 48.20; H, 3.04; F, 9.54; N, 7.02. Found: C, 50.15; H, 3.34; F, 9.17; N, 6.77.

1. customTo a 500 ml, 4-necked flask fitted with a stirrer
2. additionthermometer, addition funnel
3. temperaturereflux condenser
4. additionis added dropwise over a 30 minute period
5. additionTen minutes after completion of addition the reaction mixture
6. extractionthe product extracted into benzene (3×100 ml)
7. dry with materialThe combined benzene extracts are dried with anhydrous magnesium sulfate