Sodium hydride → 1-methyl-5,10-dihydrobenzo[b]pyrazolo[3,4-e][1,4]diazepin-4(1H)-one

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

Sodium (methylsulphinyl)methanide (29.7 mmol) was pre-pared from sodium hydride (60% dispersion in oil, 1.19 g, 29.7 mmol) and anhydrous dimethyl sulphoxide (7 ml) by heating at 65° C. until a solution was observed. To this was added a solution of 5-(2-amino-phenylamino)-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester from Example E11.2 (3.63 g, 16.9 mmol) in anhydrous dimethyl sulphoxide (10 ml), and stirring continued at 65° C. for 2.5 h. The mixture was poured into ice (100 ml), and the resulting solid collected and purified by recrystallisation from methanol/EtOAc/60-80 pet ether to yield the title compound (1.46 g, 40%).

Herkunft & Nachweise