Formic Acid → HCID 44330132, compound

Participants

Reaction Steps

A mixture of formic acid (3.0 mL) and acetic anhydride (0.4 mL) premixed for 30 minutes at 0° C. was added to a solution of 0.28 g (0.58 mmol) of N-{2-[4-(2-methylquinolin-4-ylmethoxy)benzenesulfonyl]-1-(tetrahydrothiopyran-4-ylidenemethyl)ethyl}hydroxylamine (III-17) in tetrahydrofuran (4 mL) at 0° C., and stirred for another 2 hours at room temperature. After the reaction was completed, the solvent was removed under a reduced pressure, and then subjected to azeotropic distillation with toluene. The resulting residue was dissolved in a mixed solution of methanol (1 mL) and chloroform (3 mL) and stirred for 1 hour at room temperature. Then, the solvent was removed under a reduced pressure, and the obtained residue was subjected to medium pressure column chromatography on silica gel (developing solvent; chloroform:methanol=30: 1) to obtain 0.1 g (yield 34%) of the title compound as a white crystal. Its physical properties are shown below.

Provenance & Evidence