Yield: 99%

Reaction Conditions:

with bis(trichloromethyl) carbonate;Triphenylphosphine oxide in ethyl acetate at 50; for 5 h;Temperature;Solvent;

Steps:

1-27 Synthesis of isoquinoline-5-sulfonyl chloride hydrochloride
The isoquinoline-5-sulfonic acid (31.38g, 150mmol),BTC (26.71g, 90mmol), Ph3PO (6.26g, 22.5mmol),Add ethyl acetate (300mL) to a 500mL reaction flask,Heat to 50°C for 5 hours,Down to room temperature,Add dichloromethane (150mL) and stir,Suction filtration to obtain a white solid,Vacuum dry at 4050,39.22g of solid was obtained,The yield is 99%,HPLC content is 99.99%.After the filtrate is concentrated, Ph3PO is precipitated at low temperature.After washing with a small amount of petroleum ether,Suction filtration,Ph3PO (6.23g) obtained by drying can be reused.

References:

Zhejiang University of Technology;Weng Yiyi;Li Nanhui;Sun Chen CN111909088, 2020, A Location in patent:Paragraph 0046-0099