3-methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline → (R)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-6-methyl-8-phenyl-5,6,7,8-tetrahydropyrimido[5,4-f][1,4]oxazepin-2-amine

Temperatur

120 °C

Purpose: to examine scale-up of microwave conditions established in a previous experiment. Charged a round-bottom flask with a mixture of 3-methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline (0.702 g, 3.45 mmol), (R)-2-chloro-6-methyl-8-phenyl-5,6,7,8-tetrahydropyrimido[5,4-f][1,4]oxazepine (1.0 g, 3.63 mmol), palladium (II) acetate (0.023 g, 0.10 mmol), rac-BINAP (0.108 g, 0.17 mmol), potassium carbonate (0.716 g, 5.18 mmol), and toluene (20 mL). The atmosphere s inerted through nitrogen purge cycles, then heated at 120 °C or 16 hours. HPLC-UV shows the reaction is not as clean as in the microwave, and conversion is very poor. The contents were allowed to continue heating over the weekend, but although conversion improved, the mixture contained many impurities. Not progressed. name='[Samples]' index='0' field='Samples' type='field' length='9'/>ber-coloured foam.

ORD-Eintrag

ord-b814b75406f3451f844066ae5ac468ab

Quelldatensatz

750 AstraZeneca ELN dataset

Originallink

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