Sulfuric Acid → 2-Amino-3,6-dichloro-5-trifluoromethylpyridine

Temperature

0 °C

In a 200 ml four necked flask equipped with a thermometer, a stirrer and a reflux condenser were placed 7 g of 2-amino-5-trifluoromethyl-6-chloropyridine, 10 ml of carbon tetrachloride and 70 ml of 20% sulfuric acid to give a homogeneous solution. Chlorine gas was introduced thereinto while cooling the flask at 0° C., and the reaction was carried out for 4 hours. After confirming the completion of the reaction by thin layer chromatography, the reaction product was poured into ice water and neutralized with a potassium hydroxide solution. 50 ml of methylene chloride was added thereto, followed by washing with water. The organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated off. The solid thus obtained was washed with n-hexane to obtain 6.7 g of the desired product.

1. customto give a homogeneous solution
2. customthe completion of the reaction by thin layer chromatography
3. washby washing with water
4. dry with materialThe organic phase was dried over anhydrous sodium sulfate
5. customthe solvent was evaporated off
6. customThe solid thus obtained
7. washwas washed with n-hexane

ORD record

ord-d1e3e5ba25ee44f0a01ee7856fb5cd25

Source dataset

uspto-grants-1982_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04349681