反应详情

温度

85 °C

A mixture of 2-Methylene-4-morpholin-4-yl-4-oxo-butyric acid (3.98 g, 20 mmol) and isobutyl-sulphinic acid (2.44 g, 20 mmol) were suspended in anhydrous toluene (80 mL) and anhydrous acetonitrile (20 mL). This mixture was warmed to 85° C. and stirred vigorously for 4.5 h. The reaction mixture was allowed to cool to room temperature and concentrated under vacuum. The residue was purified by flash chromatography using a 90 g silica gel column eluting with 10% methanol/CH2Cl2. Recovered 3.7 g of product as an oil. Triturated residue with isopropanol (5 mL)/ether (100 mL). Product began to precipitate out. Cooled this to 5° C. for 17 hrs(overnight). Product was collected by filtration, washed with ether and dried under vacuum to give 2-(2-Methyl-propane-1-sulfonylmethyl)-4-morpholin-4-yl-4-oxo-butyric acid as a white solid (1.8 g).

1. temperatureto cool to room temperature
2. concentrationconcentrated under vacuum
3. customThe residue was purified by flash chromatography
4. washeluting with 10% methanol/CH2Cl2
5. customRecovered 3.7 g of product as an oil
6. customto precipitate out
7. temperatureCooled this to 5° C. for 17 hrs(overnight)
8. filtrationProduct was collected by filtration
9. washwashed with ether
10. customdried under vacuum