(R)-6-氟-茚满-1-胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Purge a 12 L 3-necked flask with nitrogen, and then assemble thermocouple, heating mantle and condenser. Charge (1R)-6-fluoro-2,3-dihydro-1H-inden-1-amine (386 g, 2.55 mol) to the flask, add 3A-EtOH (3.9 L), diisopropylethylamine (1.34 L, 7.68 mol), and 2,6-dichloro-3-nitropyridine (643 g, 3.07 moles). Stir the reaction mixture at ambient temperature for eight hours followed by heating to 70° C. for 12 hours. Cool the reaction mixture to 8° C. over 1.25 h, then filter onto a polypropylene pad. Wash the solids with 3A-EtOH (760 mL), transfer to a tared dish and further dry in a vacuum oven (45° C.) to afford the title compound as an orange solid (786 g, 71%, 98.0% ee). GC/MS (m/z): 307 (M+). Purge a 12 L 3-necked flask with nitrogen heating mantle and condenser by heating to 70° C. for 12 hours Cool the reaction mixture to 8° C. over 1.25 h filter onto a polypropylene pad Wash the solids with 3A-EtOH (760 mL), transfer to a tared dish further dry in a vacuum oven (45° C.)