反应详情

A suspension of 0.5 g. of sodium hydride (washed free of mineral oil) in 15 ml. of tetrahydrofuran was cooled to -20° C. and stirred. To the cold stirred suspension was added in one portion 3.0 g. of methyl 3-(3-trifluoromethylphenyl)-4-amino-5-isothiazolecarboxylate. The reaction mixture was warmed to room temperature, at which time 1.5 ml. of methyl iodide was added in one portion. The reaction mixture was stirred at ambient temperature for two hours, and then was added to 50 ml. of ice water. The aqueous mixture was extracted several times with diethyl ether. The ethereal extracts were combined, washed with water, dried and the solvent was removed by evaporation under reduced pressure to afford 2.0 g. of methyl 4-methylamino-3-(3-trifluoromethylphenyl)-5-isothiazolecarboxylate.

1. additionA suspension of 0.5 g
2. stirringTo the cold stirred suspension
3. additionwas added in one portion 3.0 g
4. stirringThe reaction mixture was stirred at ambient temperature for two hours
5. additionwas added to 50 ml
6. extractionThe aqueous mixture was extracted several times with diethyl ether
7. washwashed with water
8. customdried
9. customthe solvent was removed by evaporation under reduced pressure
10. customto afford 2.0 g