반응 #294
ord-3925d0a898bc49db9d7ff1cb2ec90b8d
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실험 절차
8-chloro-2-cyclopropyl-4,5-dimethyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (122 mg, 0.48 mmol), 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (99 mg, 0.48 mmol), Pd2dba3 (11.05 mg, 0.01 mmol), BINAP (15.03 mg, 0.02 mmol) and SODIUM TERT-BUTOXIDE (69.6 mg, 0.72 mmol) were weighed in to a microwave vial, the vial was capped and flushed with argon. toluene (4 mL) was added and the mixture was heated to 100°C in a microwaver apparatus for 2 h. The cooled reaction mixture was diluted with dichloromethane and filtered. The mixture was concentrated and purified by column chromatography on Silica, using gradient elution with increasing concentration of methanol, from 0 to 8 %, in dichloromethane to give a mixture of the two diastereomers. This was then subjected to diastereo and enantio separation to give 31 mg of isomer 1, 32.6 mg of isomer 2, 29 mg of isomer 3 and 29.7 mg of isomer 4 of 2-cyclopropyl-N-(6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-yl)-4,5-dimethyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepin-8-amine (Total Yield 122.3 mg, 60 %).