Synthetic method of 2-cyano-4'-methyl diphenyl
A technology of methyl biphenyl and synthesis method, applied in the field of chemistry, can solve the problems of many by-products, difficult separation of main products, unstable yield, etc., and achieve the effect of less by-products, low toxicity and cheap raw materials
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Embodiment 1
[0031] The synthetic method of 2-cyano-4'-methylbiphenyl comprises the following steps:
[0032] 1) In a 500ml four-necked bottle, pass N 2 Replace the air in the bottle, repeat 3 times until the air is completely replaced; add o-bromobenzonitrile (50.96 g, 0.28mol) and 250ml tetrahydrofuran in sequence;
[0033] 2) Add 3mmol of catalyst, heat to 45°C under stirring, and continue stirring for 5min,
[0034] Described catalyst is Pd complex catalyst, and its structural formula is:
[0035] ;in, DBC The structure of Ph- is , R is benzhydryl. .
[0036] 3) P-bromotoluene (37.5g, 0.22mol) was slowly dropped into the solution for 0.5~1 hour. The molar ratio of p-bromotoluene to o-bromobenzonitrile is: p-bromotoluene:o-bromobenzonitrile=1:1.27; stir at 45°C for 3h;
[0037] The amount of catalyst added is: catalyst: p-bromotoluene = 0.014:1, molar ratio.
[0038] 4) Cool to room temperature, add 1.5mol / L dilute hydrochloric acid to adjust to pH=6~7; separate the organic l...
Embodiment 2
[0041] 1) In a 500 ml four-necked bottle, pass through N 2 Replace the air in the bottle, repeat 3 times, until the air is completely replaced; add o-bromobenzonitrile (25.48 g, 0.14 mol) and 250ml tetrahydrofuran successively;
[0042] 2) Add 3mmol of catalyst, heat to 30°C under stirring, and continue stirring for 10min,
[0043] Described catalyst is Pd complex catalyst, and its structural formula is:
[0044] ;in, DBC The structure of Ph- is, R is propyl.
[0045] 3) P-bromotoluene (17.1 g, 0.1 mol) was slowly dropped into the solution, and the dropping time was 0.5~1 hour. The molar ratio of p-bromotoluene to o-bromobenzonitrile is: p-bromotoluene:o-bromobenzonitrile=1:1.4; stir at 30°C for 4 h;
[0046] The amount of catalyst added is: catalyst: p-bromotoluene = 0.03:1, molar ratio.
[0047] 4) Cool to room temperature, add 1mol / L dilute hydrochloric acid to adjust to pH=6~7; separate the organic layer;
[0048] 5) Extract the aqueous layer with n-hexane (150ml ×...
Embodiment 3
[0050] 1) In a 500 ml four-necked bottle, pass through N 2 The air in the replacement bottle was repeated 3 times until the air was completely replaced; o-bromobenzonitrile (81. 9 g, 0. 45 mol ) and 250 ml of tetrahydrofuran were added successively,
[0051] 2) Add 12mmol of catalyst, heat to 60°C under stirring, and continue stirring for 8min,
[0052] Described catalyst is Pd complex catalyst, and its structural formula is:
[0053] ;in, DBC The structure of Ph- is , R is ethyl.
[0054] 3) p-bromotoluene (42.75 g, 0.25 mol) was slowly dropped into the solution for 0.5~1 hour. The molar ratio of p-bromotoluene to o-bromobenzonitrile is: p-bromotoluene:o-bromobenzonitrile=1:1.8; stir at 60°C for 2 h;
[0055] The amount of catalyst added is: catalyst: p-bromotoluene = 0.048:1, molar ratio.
[0056] 4) Cool to room temperature, add 2.5mol / L dilute hydrochloric acid to adjust to pH=6~7; separate the organic layer;
[0057] 5) Extract the aqueous layer with n-hexane (1...
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