Synthesis method of compound 1-(2-halogenophenyl)-3-methyl-butanone-1
A synthesis method and halophenyl technology are applied in the field of organic chemical synthesis, which can solve the problems of not meeting the requirements of green chemistry, inability to apply, and many side reactions, and achieve the effects of low cost, few side reactions and high product quality.
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Embodiment 1
[0020] Embodiment 1, the synthesis of 1-(2-chlorophenyl)-3-methyl-butanone-1
[0021] (1) Synthesis of 2-chloro-N-methoxy-N-methylbenzamide
[0022] In a round bottom flask, add 2-chlorobenzoic acid (15.65g, 0.1 mol), N-methoxymethylamine (18.3g, 0.3 mol), anhydrous toluene (200ml), cool to about 0°C in an ice bath, Add the toluene solution of phosphorus trichloride (phosphorus trichloride 6.878g, 0.05 mol, toluene 100 ml) dropwise, stir for 30 minutes, then warm up to room temperature, react for 2 hours, then heat up to about 60°C, continue to react for 30 minutes ; After the reaction, add saturated NaHCO to the reaction mixture 3 The solution was quenched, extracted with ethyl acetate (3 × 200 mL), the organic phases were combined, MgSO 4 Dry, filter, concentrate, and purify by column chromatography to obtain 2-chloro-N-methoxy-N-methylbenzamide. 19.5 g, yield 97.7%.
[0023] 1 HNMR (400 MHz, CDCl 3 ): δ (ppm): 7.42~7.28 (m, 4H), 3.47 (s, 3H), 3.39 (s, 3H).
[0024] (...
Embodiment 2
[0028] Embodiment two, the synthesis of 1-(2-fluorophenyl)-3-methyl-butanone-1
[0029] (1) Synthesis of 2-fluoro-N-methoxy-N-methylbenzamide
[0030] In a round bottom flask, add 2-fluorobenzoic acid (163.6g, 1mol), N-methoxymethylamine (183g, 3mol), anhydrous toluene (600ml), cool to about 0°C in an ice bath; Add the toluene solution of phosphorus trichloride dropwise (phosphorus trichloride 0.5mol, toluene 100 ml), react for 30 minutes, then raise the temperature to room temperature and react for 2 hours, then raise the temperature to 60 o C for 30 minutes; after the reaction, add saturated NaHCO 3 The solution was quenched, extracted with ethyl acetate (3 x 5 mL), the organic phases were combined, MgSO 4 Dry, filter, concentrate, and purify by column chromatography to give 2-fluoro-N-methoxy-N-methylbenzamide 。 211.48g, yield 98.9%.
[0031] 1 HNMR (400 MHz, CDCl 3 ): δ (ppm): 7.45~7.39 (m, 2H), 7.38~7.19 (m, 1H), 7.18~7.08 (m, 1H), 3.53 (S, 3H), 3.35 (S, 3H); 13 CN...
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