反応 #70332

ord-e11359836efc46f7bb1616627374d8f2

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the solvent was evaporated
  2. 2
    その他the solid obtained
  3. 3
    抽出extracted with CHCl3
  4. 4
    その他The crude mixture was purified over a SCX cartridge

実験手順

The solid residue obtained in step A was dissolved in ethanol (5 ml) and aqueous solution 2N NaOH (0.67 ml) was added. The mixture was heated at 60° C. for 2 hours, the solvent was evaporated and the solid obtained was suspended in water. The pH was taken to 6.5 and extracted with CHCl3. The crude mixture was purified over a SCX cartridge eluting with MeOH/NH3 10:1 affording 0.070 g (yield 29%) of the expected product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08536165B2uspto-grants-2013_09