Water → HCID 67146901, Verbindung

To an ice-cooled solution of ethyl diethylphosphonoacetate (0.81 g, 3.6 mmol) in tetrahydrofuran (10 mL) was added 60% sodium hydride (0.14 g, 3.4 mmol), and the mixture was stirred for 30 min. A solution of 4-[[methyl(4-phenyl-2-thiazolyl)amino]methyl]benzaldehyde (0.80 g, 2.6 mmol) in tetrahydrofuran (10 mL) was added dropwise. The mixture was stirred at room temperature for 3 hrs, water was added, and the mixture was extracted with ethyl acetate. The extract was dried and concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=18:1) to give the title compound (0.96 g, yield 98%) as a powder.

1. stirringThe mixture was stirred at room temperature for 3 hrs
2. extractionthe mixture was extracted with ethyl acetate
3. customThe extract was dried
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=18:1)

ORD-Eintrag

ord-35b12e7b9c9a45c0adfbdb0be28f073f

Quelldatensatz

uspto-grants-2011_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07960369B2