Isopropanol → HCID 21995891, compound

Participants

Reaction Steps

To a solution of 7-(4-ethoxyphenyl)-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (2.5 g) in THF (200 ml) was added at room temperature methane sulfonic acid (0.29 ml), and the mixture was stirred for 0.5 hours. To the mixture was added 2-propanol, and the mixture was concentrated under reduced pressure. Precipitated crystals were dissolved at 90° C. in 2-propanol, and the mixture was cooled to room temperature and then cooled to 0° C. to give crystals, which were collected by filtration and washed with diethylether to give colorless crystals of 7-(4-ethoxyphenyl)-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide methane sulfonate (Compound 58) (2.56 g).

Provenance & Evidence