Ammonium Chloride → HCID 21189060, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of methylmagnesium bromide (30 ml, 90 mmol, 3M solution) dissolved in tetrahydrofuran (15 ml), a solution of compound (16) (4.5 g, 30 mmol) dissolved in tetrahydrofuran (10 ml) was slowly added dropwise at −78° C. When the dropping was completed, was slowly heated to −40° C., and stirred for 5 hours. After heating to 0° C., the solution was stirred for one hour, and then, ammonium chloride (50 ml) was slowly added dropwise thereto. The reaction solution was extracted with organic solvent, washed, dried and purified by using column chromatography (eluent: hexane/ethyl acetate=10/1) to obtain 4.0 g (80%) of pure compound (17).

Provenance & Evidence