Methanesulfonic Acid → HCID 22620737, compound

Participants

Reaction Steps

The procedure is carried out as in Example 1, but starting with 2.38 g of bromine in 5 ml of acetic acid, 3.2 g of 7-trifluoromethyl-2,3,4,5-tetrahydro-1H-[1]benzazepine and 5 g of potassium thiocyanate in 35 ml of acetic acid. The brown-yellow oil isolated is chromatographed on a silica gel, eluting with ethyl acetate. A yellow oil is obtained which is dissolved in 15 ml of isopropyl ether to which there is added 1 ml of a 1.94 N solution of methanesulphonic acid in isopropanol. The white precipitate formed is filtered off and then dried under vacuum (70 Pa) at 50° C. 0.7 g of 2-imino-9-trifluoromethyl-4,5,6,7-tetrahydro-2H-thiazolo[5,4,3-jk][1]benzazepine methanesulphonate is thus obtained in the form of a white solid melting at 226° C. [analysis C13H15F3N2O3S, % calculated C 42.38, H: 4.1, F: 15.2, N: 7.5, O: 13.3, S: 17.41, % found C: 42.4, H: 3.9, F: 15.2, N: 7.5, S: 17.4].

Provenance & Evidence