Triethylamine → HCID 178510460, Verbindung

HRID 655713

Reaktionsgleichung

Reaktionsgleichung von HRID 655713
[N+:1]([C:4]1[CH:15]=[C:8]2[C:9]([O:11][C:12](=O)[NH:13][C:7]2=[CH:6][CH:5]=1)=O)([O-:3])=[O:2].C(#N)C([CH2:19][C:20]#[N:21])O.C([N:25](CC)CC)C>CN(C=O)C>[NH2:25][C:12]1[C:19]([C:20]#[N:21])=[C:9]([OH:11])[C:8]2[C:7](=[CH:6][CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:15]=2)[N:13]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 208212H-3,1-Benzoxazine-2,4(1H)-dione, 6-nitro-HCID 212535622-Hydroxybutanedinitrile

Produkt 1

HCID 178510460HCID 178510460, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To the solution of 47.25 g of 5-nitroisatoic anhydride in 230 mL of DMF 15 g of malonitrile and 63.3 mL of triethylamine were added and the reaction mixture was stirred at 60° C. for 2 hours. The solvent was evaporated at reduced pressure and the residue was mixed with 570 mL of acetonitrile and 114 mL of concd. HCl and the solution was stirred at room temperature overnight. The precipitate was then filtered off, washed with water and ethanol to give 49.7 g of product, m.p.:>360° C. LC-MS: MH+ 231; Ret. time: 4.78 min.

Aufarbeitung

  1. customThe solvent was evaporated at reduced pressure
  2. additionthe residue was mixed with 570 mL of acetonitrile and 114 mL of concd
  3. stirringHCl and the solution was stirred at room temperature overnight
  4. filtrationThe precipitate was then filtered off
  5. washwashed with water and ethanol

Quellen und Nachweise

ORD-Eintrag
ord-ae47d282d21b4cf4b96a7e291eec24aa
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08071601B2

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