Sodium Glycinate → HCID 21189951, Verbindung

HRID 1857389Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1857389
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5](F)=[CH:4][C:3]=1[CH3:12].[NH2:13][CH2:14][C:15]([O-:17])=[O:16].[Na+:18]>CN(C=O)C.O>[Na+:18].[Cl:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([NH:13][CH2:14][C:15]([O-:17])=[O:16])=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1

Komponenten

5

Edukt 2

HCID 4684308Sodium GlycinateHCID 103524921-Chloro-4-fluoro-2-methyl-5-nitrobenzene

Produkt 1

HCID 21189951HCID 21189951, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a stirred solution of 2-chloro-5-fluoro-4-nitrotoluene (0.605 g, 3.19 mmol, as prepared above) in DMF (3.0 mL) at 70° C., was added dropwise, a solution of sodium glycinate (0.310 g, 3.19 mmol, Aldrich, used as received) in water (3.0 mL). The resulting suspension was stirred overnight at 70° C. The suspension was cooled to room temperature and the resulting red solid was filtered, washed with chloroform (10 mL) and dried under vacuum to give 0.360 g (46%) pure (1H NMR) title compound as a red powder; 1H NMR (DMSO-d6): δ 2.276 (s, 3H), 3.431 (d, 2H, J=4.2 Hz), 6.848 (s, 1H), 7.963 (s, 1H), 8.773 (s, 1H).

Aufarbeitung

  1. temperatureThe suspension was cooled to room temperature
  2. filtrationthe resulting red solid was filtered
  3. washwashed with chloroform (10 mL)
  4. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-314d6ce974ea4bffa417b6d0406945a1
Quelldatensatz
uspto-grants-2000_11
Patentnummer
US06147075

Notizen zur Reaktion

Wird geladen…