反応 #1832011

ord-819d2298957f449883c03c4ac753f127

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 24 h in the temperature
  2. 2
    その他range 78-80° C
  3. 3
    その他removed during the hot filtration
  4. 4
    温度The filtrate was cooled further
  5. 5
    その他product solids were isolated by filtration
  6. 6
    洗浄washed with distilled water (20 mL)
  7. 7
    その他dried under vacuum
  8. 8
    その他to yield 200 mg (32%)

実験手順

The product of Example 5, (611 mg, 1.1 mmol) was mixed with ethanol (27 mL) and concentrated hydrochloric acid (0.5 mL) and the mixture boiled under reflux for 24 h in the temperature range 78-80° C. Distilled water (20 mL) was added to the hot reaction mixture and solids removed during the hot filtration. The filtrate was cooled further and product solids were isolated by filtration, washed with distilled water (20 mL), and dried under vacuum to yield 200 mg (32%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07019009B2uspto-grants-2006_03