反应详情

A suspension of 2.05 g of n-hexyl 3,4-dihydroxy-5-nitrophenylglyoxylate and 600.8 mg of thiosemicarbazide is stirred intensively at 90° for 30 minutes. The mixture is then cooled to 40° and treated with a solution of 870.1 mg of sodium hydroxide in 15 ml of water. The solution is subsequently heated to 90° for 30 minutes, cooled to room temperature and treated dropwise with 2 ml of conc. hydrochloric acid. The crystallized-out product is filtered under suction and then dissolved in ethyl acetate. The solution is washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. There is obtained 6-(3,4-dihydroxy-5-nitrophenyl)-3 -mercapto-1,2,4-triazin-5(4H)-one of m.p. 282°-284° (from ethanol).

1. temperatureThe mixture is then cooled to 40°
2. temperatureThe solution is subsequently heated to 90° for 30 minutes
3. filtrationThe crystallized-out product is filtered under suction
4. dissolutiondissolved in ethyl acetate
5. washThe solution is washed with saturated sodium chloride solution
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. customevaporated