A kind of phenothiazine co-sensitizer and its preparation method and application
A phenothiazine and sensitizer technology, applied in the field of phenothiazine co-sensitizers and their preparation, can solve the problems of insufficient spectral response and the like
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Embodiment 1
[0037] The specific preparation method of the present embodiment phenothiazine co-sensitizer is:
[0038] (1) Synthesis of Compound 1: At room temperature, add phenothiazine (10.00 g, 50.18 mmol) in the above synthesis route into a three-necked flask, then add N,N-dimethylformamide (80 mL), and The temperature of the mixture was lowered to 0° C., sodium hydrogen (2.41 g, 100.37 mmol) was added slowly and uniformly in batches, and stirred at room temperature for 1 hour. Afterwards, n-bromooctane (19.38g, 100.37mmol. liquid at room temperature, 17.6mL) was slowly added dropwise, reacted at room temperature for 8 hours, and the concentration of the reactant was basically unchanged by thin-layer chromatography. Chloromethane (200mL) was extracted, the organic phase was dried with anhydrous sodium sulfate, filtered and then rotary evaporated under reduced pressure, the residue was purified by 200-300 mesh silica gel column chromatography (petroleum ether / ethyl acetate=100 / 1), vacuu...
Embodiment 2
[0052] The specific preparation method of the present embodiment phenothiazine co-sensitizer is:
[0053] (1) Synthesis of Compound 1: At room temperature, the phenothiazine (10.00 g, 50.18 mmol) in the above synthesis route was added to a three-necked flask, followed by adding tetrahydrofuran (150 mL), and the temperature of the mixture was lowered to 5 ℃, sodium hydrogen (2.68g, 125.5mmol) was slowly and uniformly added in batches, and stirred at room temperature for 0.8 hours. Slowly add n-bromooctane (16.47g, 85.3mmol, liquid at room temperature, 14.9mL) dropwise thereafter, react at room temperature, trace the reactant concentration by thin-layer chromatography, the reaction is complete, quench with ice water and use ethyl acetate (250mL) extraction, the organic phase was dried with anhydrous magnesium sulfate, filtered and rotary evaporated under reduced pressure, the residue was purified by 200-300 mesh silica gel column chromatography (petroleum ether / ethyl acetate=100...
Embodiment 3
[0061] The specific preparation method of the present embodiment phenothiazine co-sensitizer is:
[0062] (1) Synthesis of Compound 1: At room temperature, add the phenothiazine (10.00g, 50.18mmol) in the above synthesis route into a three-necked flask, then add N,N-dimethylformamide (200mL). The temperature of the mixture was lowered to 8° C., and sodium hydrogen (3.61 g, 150.5 mmol) was slowly and uniformly added in batches, and stirred at room temperature for 0.6 hours. Slowly add n-bromooctane (14.54g, 75.3mmol, liquid at room temperature, 13.2mL) dropwise thereafter, react at room temperature, trace the reactant concentration by thin-layer chromatography, the reaction is complete, quench with ice water and use chloroform (300mL) extraction, the organic phase was dried with anhydrous sodium sulfate, filtered and then rotary evaporated under reduced pressure, the residue was purified by 200-300 mesh silica gel column chromatography (petroleum ether / ethyl acetate=100 / 1), and...
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