反应 #1592586
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07064123B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 2-methylene-4-morpholin-4-yl-4-oxo-butyric acid (2 g, 10.03 mmol), in DMF (5 mL), 2-trifluoromethylbenzyl mercaptan (1.93 g, 10.03 mmol) and DMAP (122 mg, 1.0 mmol) was stirred at ambient temperature for 16 hours. Methanol (200 mL) and a saturated aqueous solution of Oxone® (20 g, 32.5 mmol) were added with continued stirring for 2 hours. Methanol was removed under vacuum and the aqueous residue was diluted with 200 mL of water. The crystallized product was filtered, washed with water, and dried under vacuum to yield 4-morpholin-4-yl-4-oxo-2-(2-trifluoromethyl-benzylsulfonylmethyl)-butyric acid (0.95 g) as a white solid. Methanol was removed under vacuum the aqueous residue was diluted with 200 mL of water The crystallized product was filtered washed with water dried under vacuum
来源 ID: ord-d2b151c39d9a41da90bb419d88fb61a9