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 170886-13-2 as follows., 170886-13-2
Starting material 8d 5-Iodo-2-(trifluoromethyl)pyridin-4-ol:A 250 mL round bottom flask was charged 2-(trifluoromethyl)pyridin-4-ol (prepared as described in Tyvorskii, V. I., Bobrov, D. N. Chemistry of Heterocyclic Compounds 1997, 33, 1138-9; 42.7 mmol). MeOH (45 mL) was added, and the solution was cooled to 0 0C. Potassium carbonate (6.55 g, 47.4 mmol) was added, and the resulting mixture was treated with iodine (11.37 g, 44.8 mmol) in portions over 5 minutes. The resulting mixture was allowed to stir at 0 0C, with slow warming to room temperature. After stirring at room temperature overnight, the reaction was quenched with aqueous NaS2theta3, was acidifed withHOAc (10 mL), and was extracted with EtOAc (4x). The combined organics were washed with brine, concentrated, and purified by silica gel chromatography (gradient elution; Rf in70:30 hexanes:EtOAc = 0.30) to give a pale yellow solid (2.74 g, 22%) of -90% purity. M/Z = 288. 1H NMR (400 MHz, DMSO-D6) delta ppm 7.19 (m, 1 H) 8.80 (m, 1 H) 12.43 (s, 1 H).
The chemical industry reduces the impact on the environment during synthesis 170886-13-2, I believe this compound will play a more active role in future production and life.
Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2008/59238; (2008); A1;,
Pyridine – Wikipedia,
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