Water → 2-Amino-4-nitrobenzenethiol

HRID 1896772Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1896772
F[C:2]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=1[NH2:4].O.O.O.O.O.O.O.O.O.[S-2:21].[Na+].[Na+].C(=O)(O)[O-].[Na+].O>ClCCl>[NH2:4][C:3]1[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[CH:7]=[CH:8][C:2]=1[SH:21]

Komponenten

6

Edukt 4

HCID 962WaterHCID 677852-Fluoro-5-nitroanilineHCID 73972Sodium sulfide nonahydrateHCID 516892Sodium Bicarbonate

Produkt 1

HCID 63364002-Amino-4-nitrobenzenethiolAusbeute 100,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
125 °C

Versuchsvorschrift

2-Fluoro-5-nitroaniline (1 g, 6.41 mmol), sodium sulfide nonahydrate (1.7 g, 7.05 mmol), sodium bicarbonate (600 mg, 7.05 mmol) and water (15 mL) were combined and heated in the microwave at 125° C. for 5 min. After cooling, dichloromethane was added, and the organic layer was washed with 2M aqueous hydrochloric acid and then brine. The combined organic layers were dried over anhydrous MgSO4 and evaporated to afford 1.1 g (33%) of the title compound.

Aufarbeitung

  1. temperatureAfter cooling
  2. washthe organic layer was washed with 2M aqueous hydrochloric acid
  3. dry with materialThe combined organic layers were dried over anhydrous MgSO4
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-e9c5997c6d844913b6436a312ef63ad8
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08518980B2

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