Tertiary amine photosensitizer and preparation method thereof, and photosensitive resin composition containing tertiary amine photosensitizer, and applications thereof
A technology of tertiary amine photosensitizer and photosensitive resin, applied in the application of photosensitive resin composition, tertiary amine photosensitizer, and photosensitive resin composition field, can solve the problems of sensitizer precipitation and low solubility, and achieve relative The effect of good capacitance, high sensitivity and sufficient resolution
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[0083] According to a typical embodiment of the present invention, a preparation method of the above-mentioned tertiary amine photosensitizer is provided. The preparation method comprises the following steps: 1) react raw material a and raw material b to obtain intermediate a; 2) react intermediate a and raw material c in an organic solvent containing a catalyst to obtain intermediate b; 3) react raw material d and raw material e in nitrogen Under the protection of the catalyst, the intermediate c is obtained; (4) the intermediate b and the intermediate c are obtained through the catalytic reaction of the catalyst under the protection of nitrogen to obtain the product; the reaction equation is as follows:
[0084]
[0085] In the case of knowing the above reaction scheme, the specific reaction conditions in steps 1) to 4) can be easily determined by those skilled in the art.
[0086] The reaction of step 1) can be carried out under catalyst-free and solvent-free conditions....
Embodiment 1
[0098] Component D is the preparation of the tertiary amine derivative shown in general formula (I)
[0099] (1) Preparation of intermediate a1
[0100]
[0101] Add 63 g of benzyl chloride and 100 g of triethyl phosphite into a 500 ml four-neck flask, stir and raise the temperature to 80-90° C., and react for 3 hours. GC (gas chromatography) controls to benzyl chloride less than 1%, and the reaction ends. Distill at 90°C atmospheric pressure to remove the reaction by-product ethyl chloride, continue to distill under reduced pressure to remove unreacted triethyl phosphite, after no fraction is removed, cool down to 30°C to obtain 105g of intermediate a1 with a yield of 92.1% .
[0102] The structure of intermediate a1 via 1 H-NMR and LCMS confirmed.
[0103] 1 H-NMR (CDCl 3 , 500MHz): δ1.11 (6H, m), δ3.57 (4H, s), δ5.33 (2H, s), δ7.06-7.14 (5H, m).
[0104] MS (m / z): 229 (M+1).
[0105] (2) Preparation of intermediate b1
[0106]
[0107] Add 114g of intermediat...
Embodiment 2
[0124] (1) Preparation of intermediate c2
[0125]
[0126] Add raw materials 162.5g d2, 2-ethyl-6-methylaniline 216g, toluene 400g in a 1000mL four-necked flask, add sodium tert-butoxide 40g, tri-tert-butylphosphine 36g and tetrakis(triphenyl Phosphine)palladium 1.6g, heat up to 80-85°C and keep it warm for 10h, and control in HPLC until the reaction of raw material d2 and its intermediate monosubstituted product is complete (HPLC: <0.1%). Filtrate while hot, distill off the solvent from the mother liquor under reduced pressure, add 200 g of n-hexane, cool to 10° C., stir and crystallize, and filter with suction to obtain 197.1 g of intermediate c2 with a purity of 91%.
[0127] The structure of product 1 was determined by LCMS and 1 H-NMR confirmed.
[0128] 1 H-NMR (CDCl 3 , 500MHz): δ1.24-2.59 (16H, m), δ4.01 (2H, s), δ6.28-7.15 (12H, m), δ10.1 (1H, s).
[0129] MS (m / z): 434 (M+1).
[0130] (2) Preparation of product 2
[0131]
[0132] Add 208g of intermedia...
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