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ChemicalBook CAS DataBase List Thioxanthen-9-one

Thioxanthen-9-one synthesis

13synthesis methods
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Yield:492-22-8 99%

Reaction Conditions:

with tert.-butylnitrite;oxygen;acetic acid;2,3-dicyano-5,6-dichloro-p-benzoquinone in 1,2-dichloro-ethane at 20; for 12 h;Sealed tube;Irradiation;

Steps:

1-8 Example 1: Preparation of thioxanthone (formula (2-1))

In a 15 mL sealed tube equipped with a magnetic stirrer, 1 mmol of thioxanthene (formula (1-1)) and 0.01 mmol of DDQ were added, the air inside the tube was replaced with oxygen, and the oxygen balloon was inserted after sealing the bottle with a rubber stopper. Then, 0.05 mmol of TBN, 0.2 mmol of acetic acid and 5 mL of 1,2-dichloroethane were injected into the sealed tube, and the mixture was reacted at room temperature for 12 hours under irradiation with a 18 W blue LED lamp, and then the solvent was distilled off under reduced pressure, and then the column was further evaporated. Chromatography separation, using a mixture of ethyl acetate / petroleum ether in a volume ratio of 1:50 as an eluent, collecting the eluate containing the target compound, and evaporating the solvent to obtain the product thioxanthone, the isolated yield was 99%. .

References:

CN109232525,2019,A Location in patent:Paragraph 0024-0039

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