Methanol → 2,3-methylenedioxy-11-oxo-11H-pyrido[2,1-b]quinazoline-6-carboxylic acid

HRID 2419015

Reaktionsgleichung

Reaktionsgleichung von HRID 2419015
[NH2:1][C:2]1[CH:11]=[C:10]2[O:12][CH2:13][O:14][C:9]2=[CH:8][C:3]=1[C:4]([O:6]C)=O.Cl[C:16]1[N:24]=[CH:23][CH:22]=[CH:21][C:17]=1[C:18]([OH:20])=[O:19].CO>CN(C=O)C>[CH2:13]1[O:12][C:10]2[CH:11]=[C:2]3[C:3]([C:4](=[O:6])[N:24]4[CH:23]=[CH:22][CH:21]=[C:17]([C:18]([OH:20])=[O:19])[C:16]4=[N:1]3)=[CH:8][C:9]=2[O:14]1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 762582-Chloronicotinic acidHCID 290838Methyl 6-amino-1,3-benzodioxole-5-carboxylate

Produkt 1

HCID 203168392,3-methylenedioxy-11-oxo-11H-pyrido[2,1-b]quinazoline-6-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 2.00g (10.4 mmol) of methyl 2-amino-4,5-methylenedioxybenzoate, 1.67g (10.4 mmol) of 2-chloronicotinic acid and 50mg of KI was heated at 170° for 1 hour. The fusion or melt gradually solidified to an orange cake. The solid material was heated in boiling methanol (250 ml) and then filtered to yield 1.60g of crude product, mp. 273°-280° dec. The analytical sample was obtained by recrystallization from DMF, mp. 300°-304° dec.

Aufarbeitung

  1. temperaturewas heated at 170° for 1 hour
  2. temperatureThe solid material was heated
  3. filtrationfiltered
  4. customto yield 1.60g of crude product, mp. 273°-280° dec

Quellen und Nachweise

ORD-Eintrag
ord-6c4ebe5621724a688721fa60eaf7865f
Quelldatensatz
uspto-grants-1978_08
Patentnummer
US04104389

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