1-(4-Bromophenyl)cyclopropane-1-carbohydrazide → 3-[1-(4-Bromophenyl)cyclopropyl]-8-({[tert-butyl(dimethyl)silyl]oxy}methyl)-8-methyl-5,6,8,9-tetrahydro[1,2,4]triazolo[4,3-d][1,4]thiazepine

Participants

Reaction Steps

A solution of 7-({[tert-butyl(dimethyl)silyl]oxy}methyl)-7-methyl-5-(methylthio)-2,3,6,7-tetrahydro-1,4-thiazepine (34.4 g, 108 mmol) and the compound (27.5 g, 108 mmol) obtained in Example 16-3) in 1-butanol (800 mL) was stirred at 140° C. for 6 h. The reaction mixture was cooled to room temperature, the solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1 to 1:0) to obtain the title compound (36.3 g, 66%) as a white solid.

Provenance & Evidence