Oxime ester compound and its production method
A compound and oxime ester technology, applied in the field of functional material research, can solve the problems of unfavorable commercialization, difficult synthesis, complex structure, etc., and achieve the effects of less three wastes, stable product quality, and high content
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[0128] The present invention is further described in detail below by way of examples.
Synthetic example 1
[0130] Step 1: Synthesis of ethyl 2-cyano-3-(4-dimethylamino-phenyl)-N-hydroxyacrylimide (compound 1-1)
[0131]
[0132] In a 250mL three-neck flask with a thermometer and a stirrer, add 12.2g of 2-cyano-3-(4-dimethylamino-phenyl)-ethyl acrylate, 4.0g of hydroxylamine hydrochloride, and 5.33 g of anhydrous sodium acetate in sequence. g, 100mL of absolute ethanol, heated to reflux for 5h, cooled to room temperature, then poured into 300g of ice water, stirred, filtered, and dried to obtain 2-cyano-3(4-dimethylamino-phenyl)- N-hydroxyacrylimide ethyl ester (compound 1-1) 12.38g, yield: 95.5%. As determined by HPLC, content: 98.3%. MS(EI): 259.13; Calculated for elemental analysis C 14 h 17 N 3 o 2 (%): C 64.85, H 6.61; Found: C 64.63, H 6.72.
[0133] Step 2: Synthesis of ethyl 2-cyano-3-(4-dimethylamino-phenyl)-N-acetoxyacrylimide (compound 1)
[0134]
[0135] In a 250mL three-neck flask with a thermometer and a stirrer, add the 2-cyano-3-(4-dimethylamino-phenyl)...
Synthetic example 2
[0137] Step 1: Synthesis of ethyl 2-cyano-3-(4-dimethylamino-phenyl)-N-hydroxyacrylimide
[0138] Ethyl 2-cyano-3-(4-dimethylamino-phenyl)-N-hydroxyacrylimide (Compound 1-1) was prepared in the same manner as in Step 1 of Synthesis Example 1.
[0139] Step 2: Synthesis of ethyl 2-cyano-3-(4-dimethylamino-phenyl)-N-benzoyloxyacrylimide (compound 2)
[0140]
[0141] In a 250mL three-neck flask with a thermometer and a stirrer, add the ethyl 2-cyano-3-(4-dimethylamino-phenyl)-N-hydroxyacrylimide (compound 1-1) 9.73g, 5.68g of triethylamine, and 150mL of dichloromethane were completely dissolved and then cooled to 0°C. At 0-5°C, 7.91g of benzoyl chloride was added dropwise, and continued at this temperature after the dropwise addition was completed. Stir for 50min, then warm up to room temperature, continue to stir for 2h, then pour it into 200g of ice water, fully wash with water, separate layers, collect the organic layer, extract the aqueous layer twice with 20mL dichlorom...
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