反应详情

温度

60 °C

Thionylchloride (253 mL) was added dropwise to 3 1 methanol at 0°-10° C. Toward end of the addition, the temperature was allowed to rise to 20° C. Solid 2-nitro-3-methylbenzoic acid (500 g) was charged in one portion and the reaction mixture was heated to reflux overnight. It was distilled until pot reached 73° C. After cooling to 60° C., 685 mL water was introduced dropwise and the reaction mixture was cooled to 20° C. Upon adding 26 mL water and 125 mL 80% NaOH, the pH was adjusted to 7. The product was collected by filtration and washed with 3×100 mL water and air dried overnight. Yield of methyl 2-nitro-3-methylbenzoate was 503.5 g (93.5%), mp 72° C.

1. additionToward end of the addition
2. customto rise to 20° C
3. temperaturethe reaction mixture was heated
4. temperatureto reflux overnight
5. distillationIt was distilled
6. customuntil pot reached 73° C
7. addition685 mL water was introduced dropwise
8. temperaturethe reaction mixture was cooled to 20° C
9. additionUpon adding 26 mL water and 125 mL 80% NaOH
10. filtrationThe product was collected by filtration
11. washwashed with 3×100 mL water and air
12. customdried overnight