反应详情

While maintaining a solution comprising 27.7 g of methyl 3-amino-2-methylbenzoate, 41.5 g of sodium thiocyanate and 250 ml of methanol at a temperature of not higher than 0° C., 100 ml of sodium bromide-saturated methanol with 28.1 g of bromine was slowly dropwise added thereto. The mixture was stirred at room temperature for 3 hours and then poured into 1 liter of ice water. The solution was neutralized with sodium carbonate and then extracted with chloroform. The extract was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. Then, the solvent was distilled off to obtain 34.0 g of the desired product as an oily substance.

1. temperatureWhile maintaining a solution
2. customhigher than 0° C.
3. extractionextracted with chloroform
4. washThe extract was washed with a saturated sodium chloride aqueous solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThen, the solvent was distilled off