Nitric Acid → 4-Ethyl-3-nitroaniline

Temperature

8 °C

4-Ethylaniline (10.3 mL, 82.5 mmol) was added dropwise to sulfuric acid (96%, 63 mL), cooled to 8° C., maintaining the temperature below 10° C. After the addition, the reaction mixture was cooled to −5° C., before the addition of a mixture of nitric acid (100%, 4 mL) and sulfuric acid (96%, 10 mL), keeping the temperature below 0° C. The reaction mixture was then stirred at the same temperature for 1 h. The reaction mixture was poured into ice (200 mL) and the precipitate filtered and washed with water. The solid was suspended with water (100 mL) and neutralized with ammonium hydroxide (35%). The precipitate was filtered and dried in the oven to obtain a light-brown solid (10 g, 73%).

1. temperaturemaintaining the temperature below 10° C
2. additionAfter the addition
3. customthe temperature below 0° C
4. filtrationthe precipitate filtered
5. washwashed with water
6. filtrationThe precipitate was filtered
7. customdried in the oven

ORD record

ord-b1acf6c9f0c5498c84357022a2aa9205

Source dataset

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09284298B2