反応 #70339

ord-5f9f7668ae5242c081121df1294b9a7b

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 SiO2 eluting with DCM/MeOH 2%

実験手順

The solid residue obtained in step A was dissolved in methanol (3 ml) and aqueous solution 2N NaOH (1 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 SiO2 eluting with DCM/MeOH 2% affording 0.170 g (yield 81%) of the expected product.

出典

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