反应详情

To a solution of N-[3-(4,5,7-trifluorobenzothiazol-2-yl)-1-thioxopropyl]-N-methylglycine ethyl ester (190 mg, 0.5 mmol) in a mixture of water (3 ml) and dioxane (6 ml) was added dropwise 2N sodium hydroxide (0.6 mmol) with stirring under ice-cooling and the mixture was stirred for 1 hour at room temperature, then diluted with water and washed with ether. The aqueous phase was acidified with 7% hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water, dried and then evaporated to yield a residue, which was crystallized from isopropyl ether to give N-[3-(4,5,7-trifluorobenzothiazol-2-yl)-1-thioxopropyl]-N-methylglycine (155 mg, 88%) as a pale brown powder.

1. temperaturecooling
2. stirringthe mixture was stirred for 1 hour at room temperature
3. washwashed with ether
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with water
6. customdried
7. customevaporated
8. customto yield a residue, which
9. customwas crystallized from isopropyl ether