反応 #653770

ord-375eb5af7160439d8f8070615c47fc9c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was kept below 5° C
  2. 2
    抽出the aqueous phase was extracted with further ethyl acetate (2×500 ml)
  3. 3
    乾燥dried (MgSO4)
  4. 4
    その他evaporated in vacuo

実験手順

A solution of sodium periodate (21 g, 0.10 moles) in water (150 ml) was added slowly to a solution of (R)4-methyl-3-pyridin-2-yl-[1,2,3]oxathiazolidine-2-oxide (15.4 g, 0.78 moles) and ruthenium(III)chloride (20 mg) in acetonitrile (1540 ml) whilst the temperature was kept below 5° C. A heavy precipitate developed. The mixture was poured into a mixture of ethyl acetate (500 ml) and water (500 ml) and then shaken. The organic phase was retained and the aqueous phase was extracted with further ethyl acetate (2×500 ml). The organic phases were combined, backwashed with water (500 ml), dried (MgSO4) and then evaporated in vacuo to give (R)-4-methyl-3-(2-pyridyl)-[1,2,3]-oxathiazolidine-2,2-dioxide (15.5 g) as a yellow oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06175012B1uspto-grants-2001_01