2-chloro-4-methyl-6-phenylnicotinonitrile synthesis
- Product Name:2-chloro-4-methyl-6-phenylnicotinonitrile
- CAS Number:112190-09-7
- Molecular formula:C13H9ClN2
- Molecular Weight:228.68
4240-97-5
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112190-09-7
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Yield:112190-09-7 90%
Reaction Conditions:
with trichlorophosphate at 110; for 12 h;Inert atmosphere;
Steps:
2 Example 1: Synthesis of compound 2a.
General procedure: Add compound 1a (10.0 g, 67.5 mmol) and POCl3 (20 mL) to the round-bottomed flask, respectively.The round bottom flask was placed in an oil bath at 110 , and the reaction was stirred under reflux for 12 h under the protection of N2 (the reaction progress was monitored by TLC,Developing solvent: V ethyl acetate: V petroleum ether = 1: 4), after the reaction is completed, cool to room temperature,Remove most of the POCl3 under reduced pressure, slowly add ice water and saturated NaHCO3 solution,Adjust the pH of the solution to about 7, and transfer the mixed solution to a 500 mL separatory funnel.Extract with saturated NaHCO3 solution (3 × 30 mL) and DCM (5 × 30 mL), combine the organic phases, wash with saturated NaCl 3 to 4 times,Anhydrous Na2SO4 was dried and concentrated under reduced pressure to obtain compound 2a as a milky white powder. Yield: 95%.
References:
CN110305128,2019,A Location in patent:Paragraph 0016-0017
93-91-4
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112190-09-7
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