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

HRID 1167978

반응식

HRID 1167978 반응식
[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

참가 물질

5

반응물 3

HCID 6356Boron trifluorideHCID 678794-Fluorobenzoyl chlorideHCID 1401461-Phenylsulfonylpyrrole

생성물 1

HCID 219729051-Benzenesulfonyl-2-(4-fluorobenzoyl)pyrrole수율 33%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a solution of 4-fluorobenzoylchloride (1.74 g, 11 mmol) in dichloromethane (2 ml) 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. Yield: 19.8%.

후처리

  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

출처 및 근거

ORD 기록
ord-417490e6bfb1404886152f4839f0b2be
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620841B1

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