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CAS No. : | 131-57-7 | MDL No. : | MFCD00008387 |
Formula : | C14H12O3 | Boiling Point : | - |
Linear Structure Formula : | C6H5COOHC6H3OCH3 | InChI Key : | DXGLGDHPHMLXJC-UHFFFAOYSA-N |
M.W : | 228.24 | Pubchem ID : | 4632 |
Synonyms : |
Benzophenone 3
|
Chemical Name : | (2-Hydroxy-4-methoxyphenyl)(phenyl)methanone |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338-P304+P340-P405-P501 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With chlorosulfonic acid; In ethyl acetate; at 45℃; | Weigh 228g (1mol) 2-hydroxy-4-methoxy-benzophenone dissolved in an appropriate amount of ethyl acetate, fully stirred to dissolve, weighed 232g (2mol) of chlorosulfonic acid dissolved in an appropriate amount of ethyl acetate, The two raw materials were simultaneously pumped into the microreactor in a continuous and constant form, and the continuous reaction was carried out at 45C. The collected reaction liquid was cooled to below 5C and filtered, washed with ethyl acetate solvent, and dried at 30C under vacuum to obtain BP- 4. The yield can reach 96% |
With chlorosulfonic acid; In phthalic acid dimethyl ester; | EXAMPLE 5 11.4 g of 2-hydroxy-4-methoxybenzophenone were dissolved in 30 ml of dimethyl phthalate at 80 C., and 3.5 ml of chlorosulfonic acid were added dropwise at this temperature. Stirring was carried out for a further 4 hours at 80 C., the mixture was cooled to room temperature and 25 ml of ether were added to the solution. The precipitate was filtered off under suction, washed with ether and hexane and dried under reduced pressure at 30 C. 10 g of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid of melting point 112-114 C. were obtained (water content 7.7%). | |
With chlorosulfonic acid; at 25℃; for 20h;Inert atmosphere; Autoclave; | (1) pre-enamel kettle adding solvent and 2-hydroxy-4-methoxy benzophenone;(2) in a nitrogen atmosphere and stirred dropwise chlorosulfonic acid, water bath through the jacket cooling and control acid dropwise speed control of the autoclave temperature is 25 ;(3) chlorosulfonic acid added at the end of the reaction was continued for 20h at 25 , after the end of the reaction, the product was isolated by filtration and centrifugation;(4) with the appropriate solvent washing products, dried under nitrogen, throughout the synthesis process, the solvent used and by-products are to be recycled. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85.95 g | With sulfuric acid; water; at 110℃; for 5h; | <strong>[4065-45-6]2-hydroxy-4-methoxybenzophenone-5-sulfonic acid</strong> purified solvent concentrate 200g, purified water 200g, concentrated sulfuric acid (98%) 300g was added to a 1000ML four-necked flask at an oil bath temperature of 110 C The reaction was refluxed for 5 hours, the heating was stopped, and the mixture was cooled to reflux without reflux, and the upper aqueous phase was recovered. The lower settled oil was weighed 102.55 g.The lower layer of the precipitated oil was weighed to 102.55 g, and the mixed solvent of 1500 mL of dichloromethane and ethyl acetate in a volume ratio of 1:1.2 was placed in a 2000 ML four-necked flask. The lower layer of the precipitated oil was added to the mixed solvent, and heated to full dissolution. After 30 minutes, it was sufficiently dissolved, cooled to 23-28 C to carry out cooling crystallization, and vacuum filtration to obtain 85.95 g of 2-hydroxy-4-methoxybenzophenone wet crystal.The dichloromethane-ethyl acetate crystallization mother liquor was concentrated to recover the solvent, and the solvent was repeatedly used for treatment. After desolvation at 120 C, 100 g of ethanol was added, and after heating to complete dissolution, the crystals were cooled, and the dried weight was 18.54 g at 105 C to obtain the target product. HPLC detection purity 99.63%, |
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