반응 #55231
ord-62ae3b709edc47be93928bfc87b52c2a
반응 방정식
반응 조건
후처리
- 1온도cooling slightly
- 2workup.STIRRINGAfter the reaction mixture had been stirred for a further hour at 40° C.
- 3workup.ADDITIONit was added dropwise in the course of 30-60 minutes at 60°-80° C.
- 4온도the mixture was heated
- 5온도under reflux for 4-6 hours
- 6기타being absorbed in water
- 7온도After cooling to 60°-70° C.
- 8온도to cool (hydrogen sulfide being
- 9기타being absorbed in sodium hydroxide solution) and elementary sulfur, which
- 10기타had precipitated at the same time
- 11여과was filtered off
- 12기타the mixture was reacted at pH 1 and 50°-80° C.
실험 절차
154.5 g (1.5 moles) of sulfur dichloride were initially introduced into a stirred flask and 100 g (1.0 mole) of pinacolone were added dropwise in the course of 2 hours at 20°-40° C., whilst stirring and cooling slightly, HCl being released via the reflux condenser. After the reaction mixture had been stirred for a further hour at 40° C., it was added dropwise in the course of 30-60 minutes at 60°-80° C., whilst cooling, to 220 ml of a 40.5% strength solution of 2 moles of dimethylamine in water. A solution of 140 g (3.5 moles) of NaCH 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 reflux 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, whilst continuing to cool (hydrogen sulfide being released as a gas and being absorbed in sodium hydroxide solution) and elementary 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 mixture and could be isolated easily by filtering off.