Ammonia → HCID 131730609, compound

Participants

Reaction Steps

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

Provenance & Evidence