反応 #6910

ord-410a6f1443c34331ba6735f7cc64c911

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed twice with brine
  2. 2
    乾燥dried over sodium sulfate
  3. 3
    ろ過filtered through a fritted funnel
  4. 4
    その他the volatiles were removed under vacuum
  5. 5
    その他This provided the product, MS
  6. 6
    その他m/z 356, which was used in the next step without further purification

実験手順

A mixture of the product of Step D (60 mg; 0.1863 mmol), hydroxyl amine hydrochloride (3 eq.), sodium carbonate (4 eq.) in 1.5 mL water and 2.5 mL ethanol was heated to 90° C. for 6 h. The mixture was diluted with dichloromethane, washed twice with brine, dried over sodium sulfate, filtered through a fritted funnel and the volatiles were removed under vacuum. This provided the product, MS: m/z 356, which was used in the next step without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07084156B2uspto-grants-2006_08