[[(Aminooxy)carbonyl](methyl)amino]methane hydrochloride → [(Z)-[3-[[2-(4-fluorophenyl)-2-hydroxyethyl]-methylsulfamoyl]-5,6-dihydro-4H-1-benzothiophen-7-ylidene]amino] N,N-dimethylcarbamate

Participants

Reaction Steps

7-Oxo-4,5,6,7-tetrahydro-benzo[b]thiophene-3-sulfonic acid [2-(4-fluorophenyl)-2-hydroxyethyl]-methyl-amide (the compound of Preparation Example 48) (60 mg) and [[(aminooxy)carbonyl](methyl)amino]methane hydrochloride (the compound of Preparation Example 122) (24 mg) were stirred in acetic acid at 50° C. for 3 hours. The residue resulting from the removal of the solvent by evaporation was purified by silica gel column chromatography (hexane/ethyl acetate). Among the two spots that were identifeid by developing the reaction solution by TLC (solvent system was hexane:ethyl acetate=1:3), the fraction of the compound with a high polarity (low Rf value) was collected, and the title compound (9 mg) was obtained as a colorless amorphous substance.

Provenance & Evidence