Reaction #2068012
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06093851
Conditions: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: A solution consisting of 10 g of (RS)-1-(2,3-dichlorophenyl)ethylamine and 30 g of methyl t-butyl ether was heated to 45° C. while stirring, and a mixture of 3.6 g of L-mandelic acid and 30 g of methyl t-butyl ether was added thereto over about 30 minutes, followed by stirring at the same temperature for 30 minutes. Then, after cooled to 20° C. over 6 hours, the precipitated crystals were filtered, washed twice with 20 g of methyl t-butyl ether and dried to obtain 7.2 g of diastereomer salt. 21 g of a 5% aqueous sodium hydroxide solution was added to the crystals, followed by extraction twice with 10 g of methyl t-butyl ether. The solvent was distilled off from the resulting organic layer to obtain 4 g of (R)-1-(2,3-dichlorophenyl)ethylamine. This had the optical purity of 90.4%ee. was added by stirring at the same temperature for 30 minutes Then, after cooled to 20° C. over 6 hours the precipitated crystals were filtered washed twice with 20 g of methyl t-butyl ether dried to obtain 7.2 g of diastereomer salt followed by extraction twice with 10 g of methyl t-butyl ether The solvent was distilled off from the resulting organic layer
Source ID: ord-9b0158ab76ec4acea682a8927e4f0df2