反应详情

温度

140 °C

38 ml of water and 102 g of concentrated sulfuric acid were heated to 110° C. At 95° C., 0.25 mol of 3-amino-4-methylsulfonylbenzoic acid was added. The mixture was then heated to 140° C., and 0.8 g of sodium iodide and 0.3 mol of glycerol were added. The reaction temperature was then increased to 150° C. While the mixture was heated to and stirred at 150° C. (1 hour), 47 g of distillate were collected. After cooling, the reaction mixture was carefully admixed with 200 ml of water and diluted with a further 800 ml of water. Using 20% strength aqueous sodium hydroxide solution, the pH was adjusted to 13 and the mixture was filtered and adjusted to pH 3.5 with sulfuric acid. This procedure was repeated. A precipitate was formed which was filtered off with suction. The filtrate was adjusted to pH=2 and the resulting precipitate was filtered off with suction, washed with water and dried.

1. temperatureThe reaction temperature was then increased to 150° C
2. temperatureWhile the mixture was heated to and
3. customwere collected
4. temperatureAfter cooling
5. additiondiluted with a further 800 ml of water
6. filtrationthe mixture was filtered
7. customA precipitate was formed which
8. filtrationwas filtered off with suction
9. filtrationthe resulting precipitate was filtered off with suction
10. washwashed with water
11. customdried