Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, A new synthetic method of this compound is introduced below., Safety of 2-(2,6-Dichlorophenyl)acetonitrile
Example 9a Preparation of 2-(2,6-dichlorophenyl)-2-methylpropanenitrile To a 1 M solution of potassium tert-butoxide (403 mL, 403 mmol) at -66 C. (acetone/dry ice) was slowly added 2-(2,6-dichlorophenyl)acetonitrile (25.0 g, 134 mmol) in anhydrous THF (150 mL). The mixture was stirred at -66 C. for 20 minutes. Then, iodomethane (33.6 mL, 538 mmol) was added drop-wise over 25 minutes at -66 C. At this stage, it was exothermic and a large amount of light yellow precipitate was observed. The suspension was stirred at -60 C. for 30 minutes. The reaction mixture was quenched with 200 mL ice water, and extracted with ether (3*150 mL). The organics were combined, washed with 150 mL brine, dried over Na2SO4, and concentrated on a rotary evaporator. The crude product (30 g, yellow oil) was purified by column chromatography (ISCO, 330 g silica, 20% EtOAc in hexanes) to afford 2-(2,6-dichlorophenyl)-2-methylpropanenitrile (28.2 g, 132 mmol, 98% yield) as a light yellowish oil. 1H-NMR (CDCl3, 400 MHz) delta 7.35 (d, 2H, J=8.03 Hz), 7.16 (t, 1H, J=8.0 Hz), 2.09 (s, 6H); 13C-NMR (CDCl3, 126 MHz) delta 134.6, 133.8, 131.4, 129.0, 124.1, 38.6, 29.2; MS m/e 214.10 (M+H+); HPLC (XBridge 5mu C18 4.6*50 mm, 4 mL/min, Solvent A: 10% MeOH/water with 0.2% H3PO4, Solvent B: 90% MeOH/water with 0.2% H3PO4, gradient with 0-100% B over 4 minutes): 3.16 minutes.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; EXELIXIS PATENT COMPANY LLC; Busch, Brett B.; Stevens, JR., William C.; Kick, Ellen K.; Zhang, Haiying; Bollu, Venkataiah; Martin, Richard; Mohan, Raju; US2015/299136; (2015); A1;,
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