反应详情

Phosphorus oxychloride (POCl3) (9.65 mL, 103.5 mmol) was added to a stirred suspension of 4-chloro-7-chlorosulphonyl-1-(2H)-isoquinolone (22.1 g, 79.6 mmol) in MeCN (500 mL) at room temperature and the mixture was then heated at reflux for 15 h. On cooling, the MeCN solution was decanted from the insoluble sludge and evaporated in vacuo. The residue was extracted with hot EtOAc and evaporated to leave a solid which was stirred with Et2O (1.2 L) at room temperature overnight. The ethereal solution was decanted from the insoluble material and evaporated in vacuo to give 7-chlorosulphonyl-1,4-dichloroisoquinoline (20 g, 67 mmol) as a pale yellow solid.

1. temperaturethe mixture was then heated
2. temperatureat reflux for 15 h
3. temperatureOn cooling
4. customthe MeCN solution was decanted from the insoluble sludge
5. customevaporated in vacuo
6. extractionThe residue was extracted with hot EtOAc
7. customevaporated
8. customto leave a solid which
9. customThe ethereal solution was decanted from the insoluble material
10. customevaporated in vacuo