反应 #543578

ord-0a298d99e03a41c588c18607c8b057ee

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the solvent was evaporated in vacuo
  2. 2
    workup.DISSOLUTIONthe residue redissolved in a small volume of ethanol
  3. 3
    其他The product precipitated from the solution by the addition of ethyl acetate
  4. 4
    过滤The precipitate was collected by filtration
  5. 5
    其他dried

实验过程

A mixture of 3-hydroxybenzoic acid (1.3 g, 9.4 mmol) and a ethanolic methylamine solution (33%, 1.5 ml, 12.1 mmol) were stirred at 60° C. for 48 h, then the solvent was evaporated in vacuo, and the residue redissolved in a small volume of ethanol. The product precipitated from the solution by the addition of ethyl acetate. The precipitate was collected by filtration and dried to give the subtitled compound (1.3 g, 91%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07186718B2uspto-grants-2007_03