Ethyl Acetate → HCID 57939513, compound

Participants

Reaction Steps

To 130 ml of ethyl acetate suspension of 10.1 g of 2-(4-fluoro-2-methylphenyl)-4,4-dimethoxypiperidine and 3.18 g of L-N-acetylvaline was added 35 ml of methanol, and the mixture was heated to dissolve, and then, cooled down at room temperature. After 3.5 hours, precipitated crystals were collected by filtration, and washed with 20 ml of ethyl acetate. The obtained crystals were dried under reduced pressure. Subsequently, 50 ml of chloroform was added thereto, and the mixture was washed with 30 ml of a 2M aqueous sodium hydroxide solution and 30 ml of saturated brine, dried over magnesium sulfate and concentrated under reduced pressure. To the obtained residue was added ether, and precipitated crystals were further concentrated under reduced pressure, to give 2.94 g of (2R)-2-(4-fluoro-2-methylphenyl)-4,4-dimethoxypiperidine (optical purity:97.0% ee) as shown in Table 125 below.

Provenance & Evidence