Diethyl Ether → HCID 67195988, compound

Participants

Reaction Steps

A mixture of 503 mg of 1-tert-butoxycarbonyl-4-[2-(4-chloro-2,5-difluorophenyl)-5,7-dihydrothieno[3,4-d]pyrimidin-4-yl]piperazine, 2 ml of MeOH, and 6 ml of 4M HCl-dioxane solution was stirred at ambient temperature for 1 hour. To the reaction mixture were added 15 ml of 1M aqueous sodium hydroxide and 2 ml of diethyl ether, and the precipitate was collected by filtration, washed with water and then diethyl ether, and dried under reduced pressure. The solid obtained was dissolved in 5 ml of MeOH, here was added 2 ml of 4M HCl-dioxane solution, and the solvent was then distilled off under reduced pressure. The residue obtained was washed with EtOH-EtOAc and dried under reduced pressure to yield 423 mg of 2-(4-chloro-2,5-difluorophenyl)-4-piperazin-1-yl-5,7-dihydrothieno[3,4-d]pyrimidine dihydrochloride.

Provenance & Evidence