Reacción #1483103
ord-fdd7208ff0a44b31b55a203d930da667
Ecuación de reacción
Reactivos
Condiciones de reacción
Tratamiento posterior
- 1OtroThe solid obtained in the reaction mixture
- 2Filtraciónwas filtered under vacuum
- 3Concentraciónthe solvent concentrated
- 4workup.ADDITIONdiluted with ethyl acetate/water
- 5workup.STIRRINGstirred for 15 minutes at 25-30° C
- 6OtroThe aqueous and organic layers were separated
- 7Extracciónthe aqueous layer was extracted with ethyl acetate (2×10 mL)
- 8LavadoThe combined organic layers were washed with brine solution
- 9SecadoThe organic layer was dried over Na2SO4
- 10Concentraciónconcentrated under vacuum
Procedimiento
To a stirred solution of 3 (1 g, 3.2 mmol) in acetonitrile/water (5:5 mL) was added sodium bicarbonate (0.262 g 3.2 mmol) and followed by ethanol amine (0.5 mL, 0.5 vol) at 25-30° C. The reaction mixture was stirred for 12 h at RT; the reaction was monitored by TLC. The solid obtained in the reaction mixture was filtered under vacuum, the solvent concentrated, diluted with ethyl acetate/water and stirred for 15 minutes at 25-30° C. The aqueous and organic layers were separated, and the aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic layers were washed with brine solution. The organic layer was dried over Na2SO4 and concentrated under vacuum to afford crude 64 (0.9 g, yield: 95%) as a liquid