反应 #1876844

ord-cc91ba7f425e451d989228df5b9a3e76

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他resulting in an immediate precipitate
  2. 2
    其他the mixture was partitioned between CH2Cl2 and H2O
  3. 3
    萃取The aqueous layer was extracted with CH2Cl2 (2×)
  4. 4
    干燥The combined organic layer was dried (Na2SO4)
  5. 5
    过滤filtered
  6. 6
    其他evaporated in vacuo

实验过程

A solution of Oxone® (0.54 g, 0.88 mmol) in H2O (2 mL) was added to a 0° C. solution of 4-[(2-methylthio-ethyl)-(4-fluoro-benzyl)-amino]-N-ethyl-benzenesulfonamide (0.13 g, 0.34 mmol) in MeOH (8 mL) resulting in an immediate precipitate. After 1 h, the mixture was partitioned between CH2Cl2 and H2O. The aqueous layer was extracted with CH2Cl2 (2×). The combined organic layer was dried (Na2SO4), filtered, and evaporated in vacuo to afford 0.14 g (100%) of 4-[(2-methylsulfonyl-ethyl)-(4-fluoro-benzyl)-amino]-N-ethyl-benzenesulfonamide as a pale glass; (m+H)+ 415.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07071177B2uspto-grants-2006_07