反応 #76506

ord-87022b01755e4b0aa47613e8f5c15bb5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After removing the solvent
  2. 2
    洗浄the residue was washed with ether
  3. 3
    workup.DISSOLUTIONdissolved in water
  4. 4
    温度The flask was cooled in the freezer for 2 hours
  5. 5
    ろ過the precipitate collected by filtration
  6. 6
    洗浄washed consecutively with water and ether
  7. 7
    乾燥dried over P2O5 in vacuo

実験手順

A mixture of the product from Example 79 (0.27 g, 1.1 mmol) in 25 mL acetic acid and 10 mL acetic anhydride was stirred at room temperature for 18 hours. After removing the solvent, the residue was washed with ether, dissolved in water and then basified with saturated sodium bicarbonate. The flask was cooled in the freezer for 2 hours and the precipitate collected by filtration, washed consecutively with water and ether, and dried over P2O5 in vacuo to give the title compound (0.2 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06703391B2uspto-grants-2004_03