反应 #819357

ord-3beba905aec940398508a83e6246b3d3

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGThe mixture was stirred at room temperature for 1 hr
  2. 2
    过滤The resulting insoluble materials were filtered off
  3. 3
    浓缩the filtrate was concentrated
  4. 4
    其他The residue was purified by silica gel column chromatography (hexane/ethyl acetate=2:3)

实验过程

Under ice-cooling, to a solution of methyl 4-[[(2-phenylethyl)(4-phenyl-1,3-thiazol-2-yl)amino]methyl]benzoate (535 mg, 1.25 mmol) in tetrahydrofuran (20 mL) was added 1.5M diisobutyl aluminum hydride toluene solution (2.4 mL, 3.64 mmol). The mixture was stirred at room temperature for 2 hr and sodium sulfate 10 hydrate (1.29 g, 4 mmol) was added. The mixture was stirred at room temperature for 1 hr. The resulting insoluble materials were filtered off and the filtrate was concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=2:3) to give the title compound (409 mg, yield 81%) as a colorless oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07585880B2uspto-grants-2009_09