TBAF tetrahydrofuran → HCID 59370741, compound

(R)-N-(2-chloro-5-(2-iodo-1-(triethylsilyloxy)ethyl)phenyl)methanesulfonamide (2.2308 g) was dissolved in dehydrated THF (40 mL), and a 1 mol/L TBAF-THF solution (10 mL; manufactured by Sigma-Aldrich Co.) was added thereto. The mixture was purged with nitrogen, and then was stirred for one hour at room temperature. The reaction solution was poured into brine, and the mixture was extracted with once with ethyl acetate. The organic layer was washed once with water, and then was dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The resulting residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate 71:29→50:50), and thus the title compound (0.564 g) was obtained.

1. customThe mixture was purged with nitrogen
2. additionThe reaction solution was poured into brine
3. extractionthe mixture was extracted with once with ethyl acetate
4. washThe organic layer was washed once with water
5. dry with materialwas dried over magnesium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customThe resulting residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate 71:29→50:50)

ORD record

ord-87782fb78a4843d18a0d91a5e5201fd2

Source dataset

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08008506B2