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Example 13 1-Bromoisoquinoline A mixture of 9.0 g of 1-hydroxyisoquinoline and 40 ml of phosphorus tribromide is inserted for 15 minutes into a preheated oil bath at 135oC. The resulting 2 layers are cooled and concentrated in vacuo. The residue is treated with ice, water, and sodium carbonate. The reaction mixture is extracted with chloroform, dried over sodium sulfate and concentrated. The product is purified by column chromatography, yielding 6.8 g of pale yellow crystals, mp 41-43oC.
4-(2-monofluorophenylthio)isoquinoline-1(2H)-one[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
90%
With silver hexafluoroantimonate; In 1,2-dichloro-ethane; at 100℃; for 9h;High pressure;
At room temperature, isoquinoline-1 (2Eta)-one (10 mmol), bis(2-fluorophenyl)disulfide was sequentially added to a pressure-resistant reaction tube. Ether (10 mmol), silver hexafluoroantimonate (ll mmol) and dichloroethane (6 mL). The reaction mixture is then reacted at 100 C for 9 hours. Time. The reaction was stopped, concentrated under reduced pressure to give a crude product, and finally rinsed with a mixture of petroleum ether and ethyl acetate. Chromatography gave the corresponding product 4-(2-fluorophenylthio)isoquinolin-1(2H)-one. Yield 90%;
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