反应详情

温度

45 °C

In a 100 mL volume glass flask equipped with a stirrer, a thermometer and a dropping funnel were placed 10.1 g (38.7 mmol) of methyl 4-(3-chloropropoxy)-3-methoxybenzoate (purity: 98%) obtained in the manner described in Example II-3, 0.27 g (3.87 mmol) of sodium nitrite, and 12.5 mL of acetic acid. The resulting mixture was heated to 40-50° C. under stirring. To the reaction mixture was dropwise added slowly 16.2 g (154.8 mmol) of nitric acid (60 wt. %), and the mixture was kept at the same temperature for 5 hours. After the reaction was complete, 20 mL of water was added to the reaction mixture, and the aqueous mixture was cooled to 20° C., precipitating a crystalline product. The crystalline product was collected by filtration, washed successively with 30 mL of water and 30 mL of n-heptane, and dried under reduced pressure, to give 10.9 g (isolated yield: 92.0%, purity: 98% in terms of area percentage determined by high performance liquid chromatography) of methyl 4-(3-chloropropoxy)-5-methoxy-2-nitrobenzoate as a white crystalline product.

1. customIn a 100 mL volume glass flask equipped with a stirrer
2. customobtained in the manner
3. temperaturethe aqueous mixture was cooled to 20° C.
4. customprecipitating a crystalline product
5. filtrationThe crystalline product was collected by filtration
6. washwashed successively with 30 mL of water and 30 mL of n-heptane
7. customdried under reduced pressure