反应详情

温度

30 °C

To the above obtained dichloromethane layer containing (R)-3-((S)-4-(2,4-difluoro phenyl)-2-(hydroxymethyl)pent-4-enoyl)-4-phenyloxazolidin-2-one compound of formula-5, added sodium carbonate (59.4 g) followed by iodine (177.8 g) and the reaction mixture was stirred for 3 hours at 25-35° C. After completion of the reaction, the reaction mixture was quenched with 30% hypo solution and the reaction mixture was extracted with methyl tertiary butyl ether. Both organic and aqueous layers were separated and the organic layer was washed with 30% hypo solution, followed by 10% sodium chloride solution. Distilled off the solvent completely from the organic layer. Isopropanol (600 ml) was added to the obtained compound and the reaction mixture was stirred for 1½ hour at 25-30° C. Filtered the solid, washed with isopropyl alcohol and then dried to get the title compound. Yield: 65 g; Chiral purity: 99.5%

1. customAfter completion of the reaction
2. customthe reaction mixture was quenched with 30% hypo solution
3. extractionthe reaction mixture was extracted with methyl tertiary butyl ether
4. customBoth organic and aqueous layers were separated
5. washthe organic layer was washed with 30% hypo solution
6. distillationDistilled off the solvent completely from the organic layer
7. additionIsopropanol (600 ml) was added to the obtained compound
8. stirringthe reaction mixture was stirred for 1½ hour at 25-30° C
9. filtrationFiltered the solid
10. washwashed with isopropyl alcohol
11. customdried