反应详情

温度

100 °C

2-Amino-3,4,6-trifluorothiophenol (200 mg, 1.1 mmol) was dissolved in N-methylpyrrolidone (NMP, 1 ml) under a nitrogen stream. To the resultant solution was gradually added glutaric acid (127 mg, 1.1 mmol) at room temperature and the mixture was stirred at 100° C. for 6 hours. After naturally cooling, the mixture was diluted with water and extracted with ethyl acetate. The organic phase was washed with aqueous sodium bicarbonate. The alkaline phase was acidified with 10% hydrochloric acid and re-extracted with ethyl acetate. The combined organic phases were dried and then evaporated to yield a residue, which was recrystallized from acetonitrile to give 4-(4,5,7-trifluorobenzothiazol-2-yl)butanoic acid (133 mg, 44%).

1. customat room temperature
2. temperatureAfter naturally cooling
3. extractionextracted with ethyl acetate
4. washThe organic phase was washed with aqueous sodium bicarbonate
5. extractionre-extracted with ethyl acetate
6. customThe combined organic phases were dried
7. customevaporated
8. customto yield a residue, which
9. customwas recrystallized from acetonitrile