反应 #312619

ord-8d2014efa3a447e496834ff762e78c46

反应条件

温度
110°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After evaporation the residue
  2. 2
    其他was purified by preparative HPLC on reversed phase
  3. 3
    洗涤eluting with a gradient
  4. 4
    其他formed from acetonitrile/water/NEt3
  5. 5
    其他The combined product fractions were evaporated

实验过程

A mixture of 21.7 mg (0.08 mmol) (1H-indol-5-yl)-(4-isopropyl-piperazin-1-yl)-methanone (intermediate 1), 16 mg (0.16 mmol) cyclopentylmethynol (commercially available), 38.6 mg (0.16 mmol) cyanomethylenetri-n-butylphospborane in toluene was heated to 110° C. for an extended period of time. After evaporation the residue was purified by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile/water/NEt3. The combined product fractions were evaporated to yield 5.4 mg of the title compound. MS (m/e): 354.4 (MH+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07557108B2uspto-grants-2009_07