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 116332-54-8 as follows. category: amides-buliding-blocks
a 4-Fluoro-2-(2-methylthio-4-pyrimidyl)acetophenone nBuLi (10 ml of a 1.6 M solution in hexane; 12 mmol) is added at -78 C. to a solution of diisopropylamine (2.48 ml; 17 mmol) in THF (15 ml) and stirred for 5 min. 4-Methyl-2-(methylthio)pyrimidine (2 g; 14.5 mmol) dissolved in THF (2 ml) is added dropwise and stirred for 30 mm at -78 C. 4-Fluoro-N-methoxy-N-methylbenzamide (2.66 g; 14.5 mmol) is dissolved in THF (3 ml) and added slowly to the reaction mixture. The mixture is warmed to r.t. within 45 min. and poured on water and extracted with ethyl acetate three times. The combined organic phases are dried over Na2SO4 and evaporated to dryness to yield 2.5 g (65%) of yellow crystals after recrystallisation from tert.butyl methyl ether/hexane. 1H-NMR (200 MHz CDCl3): 3.00 (s, 3H): 6.30 (s, 1H); vinyl-H of enol); 7.00 (d, 1); 7.50 (dd, 2H); 8.20 (dd, 2H); 8.7 (d, 2H). Due to pH-dependent keto-enol tautomerism, signals may be duplicated.
According to the analysis of related databases, 116332-54-8, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Revesz, Laszlo; Schlapbach, Achim; US2002/49220; (2002); A1;,
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