反応 #11333

ord-fed017dcf7f8447fae2645dbb6325d21

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe mixture was stirred for 12 hours
  2. 2
    抽出extracted with ethylacetate
  3. 3
    洗浄The extract was washed with water
  4. 4
    その他dried
  5. 5
    その他The solvent was evaporated
  6. 6
    その他The obtained crude crystal
  7. 7
    その他was recrystallized from isopropylether

実験手順

To a solution of 4-fluorobenzoylchloride (1.74 g, 11 mmol) in dichloromethane (2ml) was added dropwise a solution of boron trifluoride diethyletherate (3.4 ml, 27.6 mmol) in dichloromethane (20 ml). The mixture was stirred for 10 minutes at room temperature. Subsequently, to the mixture was added dropwise a solution of 1-benzenesulfonylpyrrole (1.9 g, 9.2 mmol) in accordance with a method described in Example 8 (1) in dichloromethane (5 ml). The mixture was stirred for 12 hours. The reaction mixture was poured into ice-water and extracted with ethylacetate. The extract was washed with water and dried. The solvent was evaporated. The obtained crude crystal was recrystallized from isopropylether to give 1-benzenesulfonyl-2-(4-fluorobenzoyl)pyrrole (1.0 g) as a crystal.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07098201B2uspto-grants-2006_08