16982-21-1, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 16982-21-1 as follows.
To a boiling solution of ethyl thiooxamate (13,3 g ,10Og, 100 mmol) in ethanol (100 mL) was added l-bromo-3-methylbutan-2-one (17,6 g ,g, 106 mmol) dropwise during 15 minutes. The solution was refluxed for one hour. The solution was added to 250 mL of ice-cold water and basified with concentrated ammonia solution. This mixture was extracted twice with AcOEtethyl acetate. The organic phase was washed with brine, dried (Na2SO4) and evaporated under reduced pressure. The crude product was purified by column chromatography with dichloromethane to dichloromethane with 2% MeOH methanol to give 13,1 g (65%) of the target product: 1H-NMR-CDCl3: 7,20 (s, IH), 4,49 (m, 2H), 3,25 (m, IH), 1,42 (t, 3H), 1,35 (d, 6H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 16982-21-1, and friends who are interested can also refer to it.
Reference:
Patent; TIBOTEC PHARMACEUTICALS LTD.; MEDIVIR AB; WO2007/14921; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics