Acetic Acid → 3-Bromo-5-(trifluoromethyl)pyridin-2-amine

In a 100 ml four necked flask equipped with the same equipments as those used in Example 3 were placed 3 g of 2-amino-5-trifluoromethylpyridine and 30 ml of acetic acid to provide a homogeneous solution. 4.4 g of bromine was dropwise added thereto while cooling the flask with ice water at 10° to 20° C., and after completion of the dropwise addition, the mixture was reacted for 1 hour. The reaction product was poured into 200 ml of water, washed with an aqueous solution of sodium thiosulfate and extracted with methylene chloride. The methylene chloride layer was dried over anhydrous sodium sulfate, and the solvent was evaporated off. The solid thus obtained was washed with n-hexane to obtain 3.5 g of the desired product.

1. customto provide a homogeneous solution
2. additionafter completion of the dropwise addition
3. customthe mixture was reacted for 1 hour
4. washwashed with an aqueous solution of sodium thiosulfate
5. extractionextracted with methylene chloride
6. dry with materialThe methylene chloride layer was dried over anhydrous sodium sulfate
7. customthe solvent was evaporated off
8. customThe solid thus obtained
9. washwas washed with n-hexane

ORD record

ord-fa8e818a9a8b4f8d9aedfb219feeefc4

Source dataset

uspto-grants-1982_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04349681