Synthetic method of alpha-isopropyl-3,4-dimethoxybenzyl cyanide
A technology of dimethoxybenzene acetonitrile and dimethoxybenzene, which is applied in the field of organic synthesis, can solve the problems of unobtainable raw materials, severe reaction conditions, long synthesis route, etc., and achieves simple post-processing, short synthesis route, and reaction mild conditions
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Embodiment 1
[0021] (1) Synthesis of 3
[0022] Add 3,4-dimethoxyphenylacetic acid (10.0 g, 50.97 mmol) into a 250 mL round bottom flask, then add 50 mL of thionyl chloride to dissolve it, and reflux for reaction. After 1 h, it was detected by TLC, and the reaction was completed. The thionyl chloride was evaporated to dryness under reduced pressure to obtain a yellow oil, which was then dissolved in 20 mL of acetonitrile, added dropwise to 50 mL of ammonia water under ice bath, and reacted under ice bath conditions. After 0.5 h, it was detected by TLC, and the reaction was completed. The acetonitrile was evaporated to dryness under reduced pressure, and a white solid precipitated out, which was filtered by suction, washed with water (50 mL×3), and dried to obtain 9.29 g of white solid 3 with a yield of 93.4%. 1 H NMR (400MHz, CDCl 3 )δ6.98–6.69(m,3H),6.04(s,1H),5.53(s,1H),3.88(s,6H),3.52(s,2H).
[0023] (2) Synthesis of 2
[0024] Add 3 (9.0g, 46.11mmol) to a 250mL round bottom flask,...
Embodiment 2
[0028] (1) Synthesis of 3
[0029] Add 3,4-dimethoxyphenylacetic acid (10.0 g, 50.97 mmol) into a 250 mL round bottom flask, then add 75 mL of thionyl chloride to dissolve it, and reflux for reaction. After 1 h, it was detected by TLC, and the reaction was completed. The thionyl chloride was evaporated to dryness under reduced pressure to obtain a yellow oil, which was then dissolved in 20 mL of acetonitrile, added dropwise to 75 mL of ammonia water under ice bath, and reacted under ice bath conditions. After 0.5 h, it was detected by TLC, and the reaction was completed. The acetonitrile was evaporated to dryness under reduced pressure, and a white solid precipitated out, which was filtered by suction, washed with water (50 mL×3), and dried to obtain 9.51 g of white solid 3 with a yield of 95.6%. 1 H NMR (400MHz, CDCl 3 )δ6.98–6.69(m,3H),6.04(s,1H),5.53(s,1H),3.88(s,6H),3.52(s,2H).
[0030] (2) Synthesis of 2
[0031] Add 3 (9.0 g, 46.11 mmol) to a 250 mL round bottom fla...
Embodiment 3
[0035] (1) Synthesis of 3
[0036]Add 3,4-dimethoxyphenylacetic acid (10.0 g, 50.97 mmol) into a 250 mL round bottom flask, then add 100 mL of thionyl chloride to dissolve it, and reflux for reaction. After 1 h, it was detected by TLC, and the reaction was completed. The thionyl chloride was evaporated to dryness under reduced pressure to obtain a yellow oil, which was then dissolved in 20 mL of acetonitrile, and added dropwise to 100 mL of ammonia water in an ice bath, and reacted in an ice bath. After 0.5 h, it was detected by TLC, and the reaction was completed. The acetonitrile was evaporated to dryness under reduced pressure, and a white solid was precipitated, which was filtered by suction, washed with water (50 mL×3), and dried to obtain 39.40 g of a white solid with a yield of 94.5%. 1 H NMR (400MHz, CDCl 3 )δ6.98–6.69(m,3H),6.04(s,1H),5.53(s,1H),3.88(s,6H),3.52(s,2H).
[0037] (2) Synthesis of 2
[0038] Add 3 (9.0g, 46.11mmol) to a 250mL round bottom flask, diss...
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