Preparation method of amide compound
A technology for amide compounds and acid halides, which is applied in the field of preparation of amide compounds, can solve the problems of high price of reaction raw materials, many reaction three wastes, difficult treatment, etc., and achieves the effects of high bactericidal activity, reduced pollution, and increased safety.
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Embodiment 1
[0053]Synthesis of 2-methyl-3- (2-pentyloxy) cyclohexhene-2-allene-1-ketone -O-benzoyl (Table 1 Compound III-68)
[0054](1) 2 - [(dimethylamino) methylene] -1,3-cyclohexidone synthesis
[0055]
[0056]Add methanol (200.0 g), dimethylamine solution (112.8 g, 40%) and 1,3-cyclohexidone (56.0 g), stirred at room temperature for 30min, cooling to 0- The formaldehyde solution (88.3 g, 37%) was slowly added dropwise, stirred for 5 h, resulting in 2- [(dimethylamino) methylene] -1,3-cyclohexidone, which is directly used in the next step.
[0057](2) Synthesis of 2-methyl-1,3-cyclohexidone
[0058]
[0059]The upper reaction solution was transferred to a high pressure reactor, and a palladium carbon catalyst (5.6 g, 10%) was added, and the reaction was reacted at 2 MPa and 30 ° C. The reaction mixture was taken out, filtrate the catalyst, and 200 g of water, evaporated to the methanol, and adjusted to pH of 6 with concentrated hydrochloride. There is a large amount of solid precipitation, filtration, dryin...
Embodiment 2
[0070]Synthesis of 2-methyl-3- (2-pentyloxy) cyclohexex-2-ethin-1-ketone -O-E-2-Element (Table 1 Compound III-67)
[0071]
[0072]The intermediate 2-methyl-3- (2-pentyloxy) cyclohexhene-2-u-1-ketime (21.1 g), triethylamine (10.1 g), toluene (200 ml), The mixture was added dropwise to Gottamoyl chloride (12.1 g), and the mixture was stirred for 3 h. The reaction solution was lowered to room temperature, and then water (100 mL) was added, and stirred at this temperature for 30 min. The oil layer is removed from the intermediate 2-methyl-3- (2-pentyloxy) cyclohexhex-2-ene-1-ketone -O-aerobatut, yield: 96% (with 2-A Base -3- (2-pentyloxy) cyclohexhene-2-ene-1-ketoxime calculation).
Embodiment 3
[0074]Synthesis of 2-methyl-3- (2-pentyloxy) cyclohexhene-2-ethin-1-ketone -O-acetoacetate (Table 1 Compound III-65)
[0075]
[0076]The intermediate 2-methyl-3- (2-pentyloxy) cyclohexhene-2-u-1-ketime (21.1 g), triethylamine (10.1 g), toluene (200 ml), The acetyl chloride (7.9 g) was added dropwise, and the mixture was stirred at room temperature for 3 h. The reaction solution was lowered to room temperature, and then water (100 mL) was added, and stirred at this temperature for 30 min. Oil layer is removed from the intermediate 2-methyl-3- (2-pentyloxy) cyclohexhene-2-allene-1-ketone -O-acetate, yield: 98% (in 2-methyl) 3- (2-glutamy) cyclohexhene-2-ene-1-ketoxime calculation).
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