반응 #1790050

반응 방정식

bromine

2-amino-5-trifluoromethylpyridine

acetic acid

→

desired product

수율 78.5%

2-Amino-3-bromo-5-trifluoromethylpyridine

수율 78.5%

용매

water

반응 조건

후처리

1. 1
   기타to provide a homogeneous solution
2. 2
   workup.ADDITIONafter completion of the dropwise addition
3. 3
   기타the mixture was reacted for 1 hour
4. 4
   세척washed with an aqueous solution of sodium thiosulfate
5. 5
   추출extracted with methylene chloride
6. 6
   건조The methylene chloride layer was dried over anhydrous sodium sulfate
7. 7
   기타the solvent was evaporated off
8. 8
   기타The solid thus obtained
9. 9
   세척was washed with n-hexane

실험 절차

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.

출처