Sodium Carbonate → 4,5-Dimethylpyridin-2-amine

HRID 869889Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 869889
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([N:9]2C(=O)C3C=CC=CC=3OC2(C)C)[CH:3]=1.C([O-])([O-])=O.[Na+].[Na+]>Cl>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([NH2:9])[CH:3]=1

Komponenten

4

Edukt 2

HCID 10340Sodium CarbonateHCID 687366023-(4,5-Dimethylpyridin-2-yl)-2,2-dimethyl-2h-benzo[e][1,3]oxazin-4(3h)-one

Produkt 1

HCID 124040134,5-Dimethylpyridin-2-amineAusbeute 103,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

A solution of 3-(4,5-dimethylpyridin-2-yl)-2,2-dimethyl-2H-benzo[e][1,3]oxazin-4(3H)-one (9 g, 0.03 mol) in concentrated hydrochloric acid (100 mL) was heated at reflux overnight. The mixture was basified by saturated solution of Na2CO3 and extracted with CH2Cl2 (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4, filtered and evaporated under vacuum to give 4,5-dimethylpyridin-2-amine (3.8 g, 97%), that was directly used in the next step without further purification.

Aufarbeitung

  1. temperatureat reflux overnight
  2. extractionextracted with CH2Cl2 (100 mL×3)
  3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. customevaporated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-98f05b2c33c34d7d99ffa5c83fa8657f
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969386B2

Notizen zur Reaktion

Wird geladen…