Sodium borohydride → HCID 22563217, compound

2-Chloro-1-pyrimidin-2-ylethanone (6.15 g, 39.3 mmol) was dissolved in ethanol (125 ml) and CeCl3.7H2O (14.64 g, 39.3 mmol) was added. Stirring was continued for 10 min then sodium borohydride (1.49 g, 39.3 mmol) was added over 2 min. After 1 hr the solid was filtered and the filtrate evaporated. Sat. ammonium chloride solution (25 ml) was added followed by brine (250 ml) and the mixture adjusted to pH3-4 with 1N.HCl. Extraction with ethyl acetate (3×250 ml) afforded an amber oil which was chromatographed over silica gel (150 g) to give the product as a pale yellow oil (3.85 g)

1. filtrationAfter 1 hr the solid was filtered
2. customthe filtrate evaporated
3. additionSat. ammonium chloride solution (25 ml) was added
4. extractionExtraction with ethyl acetate (3×250 ml)
5. customafforded an amber oil which
6. customwas chromatographed over silica gel (150 g)

ORD record

ord-acbe899ca66e40dbb461152de1c95f69

Source dataset

uspto-grants-2005_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06861438B2