反应详情

0.36 g of guanidine is suspended in 30 ml of anhydrous THF under argon, and 0.40 g of 4-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzenesulfonyl chloride (WO2003048129) is added. The mixture was stirred at RT for 24 h and then the THF was distilled off. 10 ml of water were added to the residue, and the precipitate was filtered off. It was washed with 10 ml of water and dried in vacuo. The solid was then suspended in 10 ml of EA, and 10 ml of a saturated solution of HCl in diethyl ether were added. The volatile constituents were removed in vacuo, and the residue was suspended in 10 ml of EA and stirred at RT for 5 h. The precipitate was then filtered off and dried in vacuo. 0.45 g was obtained, mp 140° C. (decomposition). Rf (EA/HEP/CH2Cl2/MeOH/conc. NH3=10:5:5:5:1)=0.30 MS (ES+):412

1. distillationthe THF was distilled off
2. addition10 ml of water were added to the residue
3. filtrationthe precipitate was filtered off
4. washIt was washed with 10 ml of water
5. customdried in vacuo
6. addition10 ml of a saturated solution of HCl in diethyl ether were added
7. customThe volatile constituents were removed in vacuo
8. stirringstirred at RT for 5 h
9. filtrationThe precipitate was then filtered off
10. customdried in vacuo
11. custom0.45 g was obtained