Methylhydrazine → HCID 445990, compound

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Reaction Steps

A mixture of 0.53 ml of methyl hydrazine and 0.17 g of potassium carbonate is stirred in 5 ml of DMA at room temperature. After the addition of 0.44 g of (E)-[4-[4-(allyl-methyl-amino)-but-2-enyloxy]-2,5-difluoro-phenyl]-(4-bromo-phenyl)-methanone in 5 ml of DMA the mixture is boiled at 120° C. After filtration the filtrate is concentrated at 80° C./0.3 Torr, taken up in methylene chloride, filtered over sodium sulphate and concentrated. The residue consisting of the title compound is dissolved in ether/hexane, treated with 0.11 g of fumaric acid and stirred. After filtration and drying there is obtained 0.41 g of (E)-allyl-[4-[3-(4-bromo-phenyl)-5-fluoro-1-methyl-1H-indazol-6-yloxy]-but-2-enyl]-methyl-amine.fumarate, m.p. 135°-137° C.

Provenance & Evidence