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ChemicalBook CAS DataBase List 2-cyclopropyl-6-fluoroquinazolin-4(3H)-one
1252134-65-8

2-cyclopropyl-6-fluoroquinazolin-4(3H)-one synthesis

2synthesis methods
52548-63-7 Synthesis
5-Fluoro-2-iodobenzoic acid

52548-63-7
161 suppliers
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57297-29-7 Synthesis
Cyclopropane-1-carboximidamide hydrochloride

57297-29-7
214 suppliers
$8.00/1g

2-cyclopropyl-6-fluoroquinazolin-4(3H)-one

1252134-65-8
14 suppliers
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Yield:1252134-65-8 93%

Reaction Conditions:

with sodium carbonate in water;isopropyl alcohol at 90; for 12 h;Sealed tube;Inert atmosphere;

Steps:

13.A-13.B The preparation method of compound III-13, the steps are:

A. Add a magnetic stir bar to the reaction tube, and connect it to the vacuum device after sealing;Pump for 5 minutes and then continue to inject argon for 1 minute, repeat the above operation 3 times and completely remove the oxygen in the reaction tube; add 5 mg of chitosan-supported cuprous iodide to the reaction tube in the state of continuous argon (CSCuI) (0.00001mol), starting material I-12: (133.0mg, 0.5mmol), II-2: (89.7mg, 0.75mmol) and sodium carbonate (70.1mg, 1.25mmol), dissolved in 3mL Mixed solvent (isopropanol: water = 9:1),Stir at 90°C for 12h;B. After the reaction, the entire reaction system was filtered and washed with 20 mL of ethyl acetate.Filter and recover chitosan solid-supported cuprous iodide (CSCuI), and then evaporate and concentrate the filtrate.The residue was separated and purified by column chromatography with different ratios of ethyl acetate/petroleum ether mixed solvent.Obtained III-1395.3mg with a yield of 93%.The ratio of the ethyl acetate/petroleum ether mixed solvent is 1:1, and the column chromatography uses silica gel as the stationary phase.

References:

CN112778218,2021,A Location in patent:Paragraph 0115-0121