As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 15258-73-8, name is (2,6-Dichlorophenyl)methanol, molecular formula is C7H6Cl2O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Recommanded Product: (2,6-Dichlorophenyl)methanol
To a solution of 2,6-dichlorobenzyl alcohol (22 mg, 0.13 mmol, 1.0 eq) in tetrahydrofuran (1.5mL) was added sodium hydride (25 mg, 0.99 mmol, 7.8 eq) and the resulting reaction mixturewas stirred at 23 C. After 10 minutes a solution of 4-{5-[3-chloro-4- (dimethylcarbamoyl)phenylj -3-cyanopyridin-2-yl } piperazine- 1 -carbonyl chloride (55 mg, 0.13 mmol, 1.0 eq) in dichloromethane (1.5 mL) was added and the reaction mixture was stirred at 23C for 16 hours. The excess sodium hydride was quenched with the dropwise addition of water(0.15 mL), the mixture was concentrated and the residue was dissolved in DMSO and purified byreverse phase liquid chromatography (Gemini-NX C18, 5 jim, 30 x 100 mm column; 0-100%CH3CN/H20 gradient w/ 0.10% TFA present) to yield 2,6-dichlorobenzyl 4-{5-[3-chloro-4-(dimethylcarbamoyl)phenylj -3-cyanopyridin-2-yl } piperazine- 1 -carboxylate. ?H NMR (400MHz, CD3OD): oe 8.69 (d, J = 2.5 Hz, 1 H); 8.29 (d, J = 2.5 Hz, 1 H); 7.79 (d, J = 1.7 Hz, 1 H);7.67 (dd, J = 8.0, 1.7 Hz, 1 H); 7.48-7.33 (m, 4 H); 5.44 (s, 2 H); 3.85-3.58 (m, 8 H); 3.13 (s, 3H); 2.92 (s, 3 H). LRMS m/z (M+H) 572.2 found, 572.1 required.
With the rapid development of chemical substances, we look forward to future research findings about 15258-73-8.
Reference:
Patent; MERCK SHARP & DOHME CORP.; RUDD, Michael, T.; BRNARDIC, Edward, J.; KIM, Yuntae; MEISSNER, Robert, S.; RADA, Vanessa; STACHEL, Shawn, J.; ZERBINATTI, Celina, V.; (125 pag.)WO2017/83216; (2017); A1;,
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