Methyl iodide → 5-(S)-Azidomethyl-3-[4'-methylthio-3'-fluorophenyl]oxazolidine-2-one

5% TFA and 2.5% triisopropylsilane in DCM (4 ml) was added to 5-(S)-azidomethyl-3-[4′-triphenylmethylthio-3′-fluorophenyl]oxazolidine-2-one (0.250 g, 0.490 mmol; prepared as described above for Example 6), and the mixture stirred for 1 h at r.t. Solvent was removed under vacuum and the residue dissolved in DMF (2 ml). Iodomethane (0.046 ml, 0.735 mmol) was added followed by dropwise addition of triethylamine (0.136 ml, 0.979 mmol). The mixture was stirred at r.t. for 2 h, evaporated, and the residue purified by PTLC (50% ethyl acetate in DCM) to give the product as a white solid (0.124 g, 90%). MS (m/z): [M+H]+=283.

1. customSolvent was removed under vacuum
2. dissolutionthe residue dissolved in DMF (2 ml)
3. stirringThe mixture was stirred at r.t. for 2 h
4. customevaporated
5. customthe residue purified by PTLC (50% ethyl acetate in DCM)

ORDレコード

ord-6038df2371b44c07a7122bbbd7584c4e

出典データセット

uspto-grants-2002_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06441005B1