反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 75 °C
PROCEDURE
实验过程
99.26 g of anthranilic acid was added to 830 g of water, the resulting mixture was heated at 75° C. and 165.3 g of p-toluenesulfonyl chloride was added thereto over 30 minutes with stirring. 495 g of 28% aqueous solution of sodium hydroxide was added dropwise and the mixture was stirred at 80° C. for one hour. The reaction mixture was added dropwise to a mixed solution of 360 g of 35% hydrochloric acid and 270 g of water at 70 to 80° C. and stirred for one hour. After cooling to 30° C., the mixture was filtered, the resulting crystals were washed with water, and the wet crystals were heated and solved in 750 g of 1-propanol to obtain a solution. After cooling to a room temperature, the solution was filtered, the resulting crystals were washed with 1-propanol, and dried under a reduced pressure to obtain 175 g of N-tosyl anthranilic acid.
WORKUP
后处理
- stirringthe mixture was stirred at 80° C. for one hour
- stirringstirred for one hour
- temperatureAfter cooling to 30° C.
- filtrationthe mixture was filtered
- washthe resulting crystals were washed with water
- temperaturethe wet crystals were heated
- customto obtain a solution
- temperatureAfter cooling to a room temperature
- filtrationthe solution was filtered
- washthe resulting crystals were washed with 1-propanol
- customdried under a reduced pressure