Sodium Iodide → HCID 44129571, compound

To a mixture of 26-2 (0.622 g, 2.6 mmol) and sodium iodide (1.56 g, 10.4 mmol) in acetonitrile (7 ml) at ambient temperature in a 3-necked round bottom flask equipped with a nitrogen inlet and rubber septum was added dichlorodimethylsilane (0.63 ml, 5.2 mmol) via syringe. The resulting mixture was stirred 60 min. Saturated sodium bicarbonate solution (30 ml) was added and the mixture was extracted with ethyl acetate (2×90 ml). The combined organic fractions were washed with 10% sodium thiosulfate solution (30 ml), brine (30 ml), dried (sodium sulfate), and the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with ethyl acetate/hexane (1:6 increasing to 1:5), to give product 26-3 as a white solid, mp: 41.5°-43.5° C.

1. customequipped with a nitrogen inlet
2. extractionthe mixture was extracted with ethyl acetate (2×90 ml)
3. washThe combined organic fractions were washed with 10% sodium thiosulfate solution (30 ml), brine (30 ml)
4. dry with materialdried (sodium sulfate)
5. customthe solvent was evaporated under reduced pressure
6. customThe residue was purified by flash column chromatography on silica gel
7. washeluting with ethyl acetate/hexane (1:6 increasing to 1:5)

ORD record

ord-54e0a2e0f3af4db6af11ab0c15614ad0

Source dataset

uspto-grants-1999_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05872138