Benzenesulfonyl chloride → HCID 2838317, Verbindung

HRID 1279609Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1279609
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[C:15]1([S:21](Cl)(=[O:23])=[O:22])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[H-].[Na+].[Cl-].[NH4+]>>[C:15]1([S:21]([NH:1][C:2]2[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=2[N+:12]([O-:14])=[O:13])(=[O:23])=[O:22])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

Komponenten

5

Edukt 4

HCID 7369Benzenesulfonyl chlorideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 67865Benzenamine, 2-nitro-4-(trifluoromethyl)-

Produkt 1

HCID 2838317HCID 2838317, VerbindungAusbeute 93,6 %

Versuchsvorschrift

To a solution of 4-amino-3-nitrobenzotrifluoride (3.09 g) in THF sodium hydride (660 mg) was added. The mixture was stirred for 30 minutes at room temperature. After stirring, benzenesulfonylchloride (3.18 g) was added thereto. The mixture was stirred for 2 hours at room temperature. In addition, sodium hydride (420 mg) was added thereto. The mixture was stirred for 1 hour. The reaction mixture was acidified by adding an aqueous solution of ammonium chloride and extracted with ethyl acetate. The organic layer was washed, dried over, filtered and concentrated to give the title compound (4.86 g) having the following physical data.

Aufarbeitung

  1. stirringAfter stirring
  2. stirringThe mixture was stirred for 2 hours at room temperature
  3. stirringThe mixture was stirred for 1 hour
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed
  6. customdried over,
  7. filtrationfiltered
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-e35837fcbc704617bb81b8d2a74f6097
Quelldatensatz
uspto-grants-2002_09
Patentnummer
US06448290B1

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