反应 #52794

ord-768d75a3d4254239a33dc767b93504f8

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The reaction mixture was concentrated
  2. 2
    workup.ADDITIONEthyl acetate was added upon which a solid
  3. 3
    其他precipitated from the aqueous layer
  4. 4
    过滤The precipitate was collected by filtration
  5. 5
    洗涤washed with water and hexane

实验过程

A mixture of 103 mg 6-(4-methoxyphenyl)-2-oxindole, 95 mg 3-(2-formyl-4,5,6,7-tetrahydro-1H-indol-3-yl)-propionic acid and piperidine (3 drops) in ethanol (2 mL) was heated to 90° C. in a sealed tube and held there for 4 hrs. The reaction mixture was concentrated and acidified with 6 N hydrochloric acid. Ethyl acetate was added upon which a solid precipitated from the aqueous layer. The precipitate was collected by filtration, and washed with water and hexane to give 57 mg of 3-{2-[6-(4-Methoxyphenyl)-2-oxo-1,2-dihydroindol-3-ylidenemethyl]-4,5,6,7-tetrahydro-1H-indol-3-yl}-propionic acid as a brown solid (30%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06855730B2uspto-grants-2005_02