反应详情

温度

60 °C

Chlorosulfonic acid (35.6 mL) was added dropwise to a solution of 1-(7-bromo-3,4-dihydroisoquinolin-2(1 H)-yl)-2,2,2-trifluoroethanone obtained (25.4 g, 82.3 mmol) in chloroform (35 mL) while cooling in ice, and the mixture was stirred at room temperature for 1 hr and at 60° C. for 4 hr. After cooling, the reaction mixture was added dropwise to ice water and the mixture was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and then the desiccant was filtered off, followed by concentration under reduced pressure. The concentrate was powdered with hexane and ethyl acetate (5:1) and then collected by filtration to afford 7-bromo-2-(trifluoroacetyl)-1,2,3,4-tetrahydroisoquinoline-6-sulfonyl chloride as a pale yellow powder (22.7 g).

1. temperaturewhile cooling in ice
2. temperatureAfter cooling
3. extractionthe mixture was extracted with chloroform
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. filtrationthe desiccant was filtered off
6. concentrationfollowed by concentration under reduced pressure
7. filtrationcollected by filtration