Reaktion #169127

ord-144ba9531d5744d5aa961aa3f4d7ebf8

Reaktionsgleichung

O
water
CCOC(=O)c1nn(C)c2c1CCC(=CN(C)C)C2=O
ethyl 6-[(dimethylamino)methylene]-7-oxo-1-methyl-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate
N=C(N)N.O=C(O)O
guanidine carbonate
CCOC(=O)c1nn(C)c2c1ccc1cnc(N)nc12
title compound
Ausbeute 164.8%
CCOC(=O)c1nn(C)c2c1ccc1cnc(N)nc12
Ethyl 8-amino-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate
Ausbeute 164.8%

Lösungsmittel

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling the mixture
  2. 2
    workup.STIRRINGstirred for 30 minutes
  3. 3
    FiltrationThe precipitate was filtered
  4. 4
    Waschenwashed with water
  5. 5
    Sonstigedried

Vorschrift

To a solution of 16.62 g (60 mmol) of ethyl 6-[(dimethylamino)methylene]-7-oxo-1-methyl-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate in 0.5 L of DMF, 27 g (150 mmol) of guanidine carbonate was added. The mixture was stirred at 110° C. overnight. After cooling the mixture was poured into water (2.5 L) and stirred for 30 minutes. The precipitate was filtered, washed with water and dried to yield 26.83 g of title compound (91%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846701B2uspto-grants-2014_09