反応 #58557

ord-9728e2b86ef14aee8d8c55b6fea98cd6

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with CH2Cl2 (300 ml)
  2. 2
    抽出The organic extract
  3. 3
    乾燥was dried (MgSO4)
  4. 4
    その他purified by silica-gel chromatography

実験手順

A solution of the product from step d) (7.37 g, 20.7) mmol) in CH2Cl2 (103 ml) was added dropwise to a slurry of AlCl3 (8.26 g, 62 mmol) in CH2Cl2 (28 ml) at 22° C. After 45 minutes, the reaction mixture was poured into ice cold 2 M NaOH (100 ml) and extracted with CH2Cl2 (300 ml). The organic extract was dried (MgSO4) and purified by silica-gel chromatography using a ethyl acetate/hexanes gradient (0% to 50% ethyl acetate) to give 4 g (68%) of the subtitle compound. MS calculated for C17H17NOS+H 284, observed 284.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07423056B2uspto-grants-2008_09