3-CYANO-2,6-DIHYDROXY-4-(TRIFLUOROMETHYL)PYRIDINE

Pale yellow solid

Take potassium hydroxide 29.8g (0.53mol) input with mechanical stirring with reflux condenser 250mL four-necked flask was slowly added 100mL of methanol, stirring for stand-by 43.4 g (0.52 mol) of cyanoacetamide were charged into a flask equipped with a mechanical stirrer, constant pressure dropping funnel, drying tube and reflux condenser 500mL four-necked flask, add 150mL of methanol, mechanical stirring heating reflux, the reaction solution was changed from cloudy to light yellow transparent and added 100 g (0.54 mol) of ethyl trifluoroacetoacetate, keep the reflux state, slowly dropping the configured potassium hydroxide methanol solution, Heated to reflux reaction 24h, central control raw materials cyanoacetamide reaction is complete, Change the reflux device for the distillation device, Methanol recovery 3/4, The residue was added to cold water, cooled, adjusted with dilute hydrochloric acid PH = 3-4, stirred 0.5h, the reaction mixture was filtered, the filter cake washed with water to give the white target 2, 6-dihydroxy-3-cyano-4 - (trifluoromethyl) pyridine, dried at 80 to constant weight to give 84.5 g, yield 80.1percent, hplc 98percent.500ml round bottom flask, 84.5 g (414 mmol) of 2, 6-dihydroxy-3-cyano-4-(trifluoromethyl) pyridine, 400 grams of phosphorus oxychloride, 35 grams of catalyst, heated to reflux 20 h, central control raw material reaction is complete, change the reflux device for the distillation unit to steal excess phosphorus oxychloride, Pour into ice-water mixture, precipitated solid, dried to give white solid 79.6g, yield 79.78%.In a 500 ml round bottom flask, 84.5 g (414 mmol) of Step 1. At room temperature, 17 g of two, Dissolving A 250 ml round bottom flask was charged with 7.4 g (36.3 mmol) of 2, 6-dihydroxy-3-cyano-4-(trifluoromethyl) pyridine, 5% sodium hydroxide 100ml, ethanol 50ml, 30% hydrogen peroxide 50ml at 80-90degrees reflux 6-8 hours, after the reaction was extracted with dichloroethane, concentrated to give 6.85 g of solid, yield 85%.

Molecular Weight:204.11
XLogP3:0.5
Hydrogen Bond Donor Count:2
Hydrogen Bond Acceptor Count:6
Exact Mass:204.01466183
Monoisotopic Mass:204.01466183
Topological Polar Surface Area:73.1
Heavy Atom Count:14
Complexity:397
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes