2-NITRO-4-PROPYLACETANILIDE synthesis

Yield:99841-36-8 150 mg

Reaction Conditions:

with sulfuric acid;nitric acid at 15; for 2.5 h;Cooling with ice;

Steps:

1.1 Step 1 Preparation of I-1

Add 168g of 4-propylacetanilide into a three-necked bottle. Turn on mechanical stirring, under ice water, drip the pre-prepared mixed acid solution (mixed with 300g of concentrated sulfuric acid and 200g of 68% concentrated nitric acid), and the temperature of the dripping process is controlled below 15°C. After about 2 hours, the dripping was completed, and the dripping was completed and kept for 30 minutes. After the reaction of the raw materials was detected, the reaction solution was poured into ice water, the organic layer was extracted with toluene, washed with saturated sodium bicarbonate aqueous solution, and saturated brine to neutrality. Dry with anhydrous sodium sulfate. The solvent was removed in vacuum and crystallized with petroleum ether to obtain 150 g of I-1 for the next operation.

References:

CN112851562,2021,A Location in patent:Paragraph 0116-0118; 0121-0122