3-(METHYLTHIO)-6-PHENYL-1,2,4-TRIAZIN-5-OL synthesis
- Product Name:3-(METHYLTHIO)-6-PHENYL-1,2,4-TRIAZIN-5-OL
- CAS Number:1566-37-6
- Molecular formula:C10H9N3OS
- Molecular Weight:219.26
Yield:1566-37-6 97.7%
Reaction Conditions:
Stage #1: thiosemicarbazide;Benzoylformic acid in water; for 0.25 h;Heating / reflux;
Stage #2: with potassium hydroxide in methanol;water at 80; for 48 h;
Stage #3: methyl iodide in methanol;water at 40; for 0.5 h;
Steps:
44.1
A mixture of thiosemicarbazide (1.8 g, 0.020 mol) and benzoylformic acid (3.0 g, 0.020 mol) in water (50 mL) was heated under reflux for 15 min. Then potassium hydroxide (1.5 g, 0.027 mol) in methanol (50 mL) was added at 80° C. The reaction mixture was stirred and heated at 80° C. for 2 days. After cooling to 35° C., methyl iodide (1.4 mL, 0.022 mol) was added. The reaction mixture was stirred at 40° C. for 30 min. The mixture was concentrated. The precipitate formed was collected by filtration, washed with water, and dried under vacuum to afford the desired product (4.3 g, 97.7%). Analytical LCMS: (M+H)+=220.1.
References:
US2008/39457,2008,A1 Location in patent:Page/Page column 31
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