Iodo benzene diacetate → HCID 129849852, compound

Participants

Reaction Steps

With reference to EXAMPLE 1-1, 11 mg (0.034 mmol) of iodobenzene diacetate was added to a mixture of 10 mg (0.033 mmol) of 4-(ferrocenylmethyl)urazole and 0.5 mL of tetrahydrofuran-d8 at room temperature. The mixture was stirred for 2 hours to give the tetrahydrofuran solution of 4-(ferrocenylmethyl)-1,2,4-triazoline-3,5-dione. A tetrahydrofuran (0.5 mL) solution of 5 mg (0.013 mmol) of cholecalciferol (VD3, manufactured by Solvay Pharmaceutical, Co.) was added to the resulting solution, followed by stirring at room temperature for an hour. The reaction mixture was concentrated under reduced pressure and the residue obtained was purified by thin layer silica gel chromatography (hexane:ethyl acetate=1:2) to give 8 mg (90%) of the titled cholecalciferol/4-(ferrocenylmethyl)-1,2,4-triazoline-3,5-dione adduct (VD3-FMTAD) as a yellow oily substance.

Provenance & Evidence