Sodium Glycinate → HCID 21189951, Verbindung

HRID 1068603Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1068603
[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. additionat 70° C., was added dropwise
  2. temperatureThe suspension was cooled to room temperature
  3. filtrationthe resulting red solid was filtered
  4. washwashed with chloroform (10 mL)
  5. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-4f6bb1d1a4684a02bce3a663aa0fbcc6
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06251903B1

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