반응 #55230
ord-41e67b5d012b4f6db398161be99d910a
반응 방정식
반응 조건
후처리
- 1온도cooling slightly
- 2workup.STIRRINGAfter the mixture had been further stirred for 1 hour at 40° C.
- 3기타over the course of about 30 minutes
- 4workup.STIRRINGthe mixture was stirred for a further 30 minutes at the same temperature
- 5온도the mixture was heated
- 6온도under reflux for 4-6 hours
- 7기타being absorbed in water
- 8온도After cooling to 60°-70° C.
- 9기타being absorbed in sodium hydroxide solution) and elemental sulfur, which
- 10기타had precipitated at the same time
- 11여과was filtered off
- 12기타the mixture was reacted at pH 1 and 50°-80° C.
실험 절차
100 g of pinacolone (1 mole) were initially introduced into a stirred flask and 154.5 g (1.5 moles) of sulfur dichloride were added dropwise in the course of 2 hours at 20°-40° C., whilst stirring and cooling slightly, HCl being released via a condenser. After the mixture had been further stirred for 1 hour at 40° C., a solution of 90 g (2 moles) of dimethylamine in water (as an approximately 40% strength solution) was allowed to run in, over the course of about 30 minutes, at 60°-80° C., while cooling with water and the mixture was stirred for a further 30 minutes at the same temperature. A solution of 140 g (3.5 moles) of NaOH in 300 ml of water was then added and the mixture was heated under reflux for 4-6 hours, dimethylamine being released as a gas via the condenser and being absorbed in water. After cooling to 60°-70° C., the pH of the mixture was adjusted to 3.0 with hydrochloric acid (hydrogen sulfide being released as a gas and being absorbed in sodium hydroxide solution) and elemental sulfur, which had precipitated at the same time, was filtered off. 106 g (1.0 mole) of thiocarbohydrazide were added to the clear filtrate and the mixture was reacted at pH 1 and 50°-80° C. to give 6-tert.-butyl-3-mercapto-4-amino-1,2,4-triazin-5(4H)-one. This was very sparingly soluble in the reaction medium and could easily be isolated by filtering off. Yield: 150 g (or 75% of theory).