Reaktion #94508

Reaktionsgleichung

end product

8-Chloro-6-phenyl-4H-pyrazolo[1,5-a][1,4]benzodiazepine-2-carboxylic acid, methyl ester

HCl

→

8-Chloro-6-phenyl-4H-pyrazolo[1,5-a][1,4]benzodiazepine-2-carboxylic acid hydrochloride monohydrate

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA mixture of 1.05 g
2. 2
   Temperaturto reflux for 2 hours
3. 3
   Einengenthe mixture was concentrated in vacuo
4. 4
   Sonstigethe residue recrystallized twice from H2O/acetone/ether
5. 5
   Sonstigeto give analytically pure end product as off-white prisms

Vorschrift

A mixture of 1.05 g. (3 mmol) of the end product of Example 9 in 3 ml. acetone and 30 ml. of 1N HCl was heated to reflux for 2 hours. After cooling to room temperature, the mixture was concentrated in vacuo and the residue recrystallized twice from H2O/acetone/ether to give analytically pure end product as off-white prisms: mp 268°-269°.

Quelle