반응 #2303553

ord-938ad3f2b3c549b4a9362192758ee24b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the reaction mixture was partitioned between ethyl acetate and water
  2. 2
    세척The organic layer was washed with brine
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    농축concentrated

실험 절차

A mixture of 6.6 g of 2-benzyl-6-(3,3-ethylenedioxypyrrolidin-1-yl)pyridine and 60 ml of N,N-dimethylformamide was stirred in advance in an ice bath. 5.5 g of N-iodosuccinimide was added thereto and the resultant mixture was stirred as it was at room temperature overnight. To the reaction mixture was added 10 ml of a 1 M aqueous solution of sodium thiosulfate and the reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and then concentrated. The residue was subjected to silica gel column chromatography with 5–10% ethyl acetate/hexane, to give 6.7 g of the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07112593B2uspto-grants-2006_09