Boron trifluoride → 1-Benzenesulfonyl-2-(4-fluorobenzoyl)pyrrole

HRID 11237

反応式

HRID 11237 の反応式
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.B(F)(F)F.[C:15]1([S:21]([N:24]2[CH:28]=[CH:27][CH:26]=[CH:25]2)(=[O:23])=[O:22])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>ClCCl>[C:15]1([S:21]([N:24]2[CH:25]=[CH:26][CH:27]=[C:28]2[C:6](=[O:7])[C:5]2[CH:9]=[CH:10][C:2]([F:1])=[CH:3][CH:4]=2)(=[O:23])=[O:22])[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

5

反応物 3

HCID 6356Boron trifluorideHCID 678794-Fluorobenzoyl chlorideHCID 1401461-Phenylsulfonylpyrrole

生成物 1

HCID 219729051-Benzenesulfonyl-2-(4-fluorobenzoyl)pyrrole収率 33%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

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.

後処理

  1. stirringThe mixture was stirred for 12 hours
  2. extractionextracted with ethylacetate
  3. washThe extract was washed with water
  4. customdried
  5. customThe solvent was evaporated
  6. customThe obtained crude crystal
  7. customwas recrystallized from isopropylether

出典と根拠

ORDレコード
ord-fed017dcf7f8447fae2645dbb6325d21
出典データセット
uspto-grants-2006_08
特許番号
US07098201B2

関連ノート

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