反応 #1969

ord-4f295b3d715849a297bcad06075e2348

溶媒

反応条件

温度
45°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The THF is removed under reduced pressure
  2. 2
    抽出is then extracted with methylene chloride
  3. 3
    乾燥The organic layer is dried over anhydrous sodium sulfate
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated in vacuo

実験手順

The product of Step 1 is dissolved in 200 mL of 2:1 THF:water and to this solution is added 6 mL of acetic acid. The reaction mixture is heated at 45° C. for approximately 5 hours. The THF is removed under reduced pressure and the aqueous reaction mixture is adjusted to a pH in the range of 8 to 9 with 10% sodium carbonate and is then extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726182uspto-grants-1998_03