2-chloro-5-cyanopyridine synthesis
- Product Name:2-chloro-5-cyanopyridine
- CAS Number:33252-28-7
- Molecular formula:C6H3ClN2
- Molecular Weight:138.55
Yield:33252-28-7 80%
Reaction Conditions:
with oxygen;copper(II) trifluoroacetate in dimethyl sulfoxide at 110; for 19 h;Sealed tube;Green chemistry;
Steps:
12.2
General procedure: phenylacetic acid or its derivative (0.5mmol), Cu(TFA)2(20mmol%), urea (1.5 mmol) was added to the pressure sealed tube containing (0.75mL) of DMSO, after filling oxygen at 130 stirred for about 20h, the process by TLC and GC tracking (specifically the reaction time is determined by GC and TLC tracking results). After the raw material was observed by the GC and TLC the reaction has been completed the reaction, the reaction was removed, cooled to room temperature.To the reaction was added 20mL of ethyl acetate, washed with NaHCO3(20mL × 2), washed with saturated brine 20mL.The combined aqueous phases with ethyl acetate (20mL × 2) after stripping the combined organic phases with anhydrous sodium sulfate. The organic phase was dried by rotary evaporator spin solvent, product was purified by silica gel column, eluent ratio of ethyl acetate: petroleum ether = 50: 1. Benzonitrile obtained in a yield of 84%.
References:
Huaqiao University;Song, Qiuling;Feng, Qiang CN103772236, 2016, B Location in patent:Paragraph 0021; 0022; 0023; 0054; 0058; 0059; 0060
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