反应 #1876841

ord-e17c250301514e26be8bfcb2abe5b00e

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the excess BH3 was quenched by addition of 0.1 M HCl
  2. 2
    其他by partitioning the mixture between CH2Cl2 and NaHCO3
  3. 3
    干燥The organic layer was dried (Na2SO4)
  4. 4
    过滤filtered
  5. 5
    其他evaporated in vacuo
  6. 6
    其他the residue was purified by MPLC (CH2Cl2 to 70:30 CH2Cl2/EtOAc)

实验过程

A solution of 1 M BH3.THF/THF (6.8 mL, 6.8 mmol) was added to a solution of 4-[(2-methylthio-ethyl)-(2-methoxy-benzoyl)-amino]-benzenesulfonamide (0.51 g, 1.34 mmol) in THF (5 mL). After 18 h, the excess BH3 was quenched by addition of 0.1 M HCl; followed by partitioning the mixture between CH2Cl2 and NaHCO3. The organic layer was dried (Na2SO4), filtered, evaporated in vacuo, and the residue was purified by MPLC (CH2Cl2 to 70:30 CH2Cl2/EtOAc) to afford 0.38 g (77%) of 4-[(2-methylthio-ethyl)-(2-methoxy-benzyl)-amino]-benzenesulfonamide as a clear glass.

来源

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