Hydrochloric Acid → N-(6-Chloro-9H-beta-carbolin-8-yl)-3,4-difluoro-benzamide

To a cold (3° C.-5° C.) solution of 9-amino-7-chloro-β-carboline (2.50 g, 11.5 mmol, as prepared in example 60 above) in pyridine (130 ml) was added 3,4-diflourobenzoyl chloride (1.67 ml, 13.25 mmol). The reaction was allowed to warm to RT and stirred for 20 h before diluting the reaction with water (60 ml) and 1M NaOH (15 ml). After stirring for 3 h at RT, the pH of the mixture was adjusted to 8-9 with 1M HCl and then poured into water (250 ml). The mixture was allowed to stand for 30 min and the product was filtered to provide 3.95 g of the title compound after washing with water and drying under reduced pressure at 55° C.-60° C.

1. additionbefore diluting
2. stirringAfter stirring for 3 h at RT
3. waitto stand for 30 min
4. filtrationthe product was filtered

ORD-Eintrag

ord-d889a1d486474a2c9d89227fb90c6a89

Quelldatensatz

uspto-grants-2008_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07348336B2