Methylamine → HCID 68532585, compound

Participants

Reaction Conditions

Reaction Steps

Trichloroacetyl chloride (2.03 mL) was added to the tetrahydrofuran solution (36 mL) of the compound prepared in Example 3 (2.76 g), and the reaction mixture was stirred at 0° C. for an hour. The reaction mixture was dropped to an aqueous solution of 40% methylamine (36 mL) on ice bath, and stirred at room temperature for 30 minutes. Water was added to the reaction mixture, and the reaction mixture was extracted with ethyl acetate. The organic layer was washed by a saturated aqueous solution of sodium chloride, and dried with anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (high flash-SI, size 3 L (made in Yamazen corporation), n-hexane/ethyl acetate=60/40→35/65) to obtain a title compound (1.55 g) having the following physical data.

Provenance & Evidence