(2-Amino-5-bromophenyl)(2-fluorophenyl)methanone → 5-Bromo-2-(3,4-dimethoxyphenylsulfonamido)-2'-fluorobenzophenone

HRID 1608854Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1608854
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Br:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5].[CH3:18][O:19][C:20]1[CH:21]=[C:22]([S:28](Cl)(=[O:30])=[O:29])[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]>N1C=CC=CC=1>[Br:17][C:14]1[CH:15]=[CH:16][C:2]([NH:1][S:28]([C:22]2[CH:23]=[CH:24][C:25]([O:26][CH3:27])=[C:20]([O:19][CH3:18])[CH:21]=2)(=[O:30])=[O:29])=[C:3]([CH:13]=1)[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5]

Komponenten

4

Edukt 2

HCID 73865(2-Amino-5-bromophenyl)(2-fluorophenyl)methanoneHCID 27341833,4-Dimethoxybenzenesulfonyl chloride

Produkt 1

HCID 233687105-Bromo-2-(3,4-dimethoxyphenylsulfonamido)-2'-fluorobenzophenone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

20 g of 2-amino-5-bromo-2'-fluorobenzophenone are heated at 85° C. for 48 hours in 120 ml of dry pyridine in the presence of 20 g of 3,4-dimethoxyphenylsulfonyl chloride. The mixture is cooled, poured into ice-cold water, the solid is filtered off, the solid is extracted with AcOEt, the organic phase is washed with water, a solution of hydrochloric acid (1N), water and then saline water. After drying over magnesium sulfate and evaporating the solvent under vacuum, a solid is obtained which is recrystallized from DCM/isopropyl ether.

Aufarbeitung

  1. temperatureThe mixture is cooled
  2. additionpoured into ice-cold water
  3. filtrationthe solid is filtered off
  4. extractionthe solid is extracted with AcOEt
  5. washthe organic phase is washed with water
  6. dry with materialAfter drying over magnesium sulfate
  7. customevaporating the solvent under vacuum
  8. customa solid is obtained which
  9. customis recrystallized from DCM/isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-44acd343b15e467caa518c10ed8bfb7f
Quelldatensatz
uspto-grants-1995_03
Patentnummer
US05397801

Notizen zur Reaktion

Wird geladen…