Sulfuric acid magnesium salt (1:1) → HCID 10118352, compound

Participants

Reaction Steps

A mixture of intermediate (3) (0.0103 mol) and MgSO4 (6.2 g) in toluene (155 ml) was stirred and refluxed for 5 hours, then filtered and washed with CH2Cl2/CH3OH 1/2. The organic layer was separated, washed with K2CO3 10%, dried (MgSO4), filtered and the solvent was evaporated till dryness. The residue (3.35 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 96/4/0.1; 15–40 μm). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from 2-propanone and diethyl ether. The precipitate was filtered off and dried, yielding 1.6 g (30%) of 5-(3-chlorophenyl)-7-[(4-chlorophenyl)hydroxy(1-methyl-1H-imidazol-5-yl)methyl]-1,5-dihydro-4,1-benzothiazepin-2(3H)-one, mp. 210° C.

Provenance & Evidence