Pyridine → HCID 13246122, compound

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Reaction Steps

In 30 g of dry benzene were dissolved 2.6 g of 4,6,6,-trichloro-3,3-dimethyl-5-hexenoyl chloride and 2.0 g of 3-phenoxybenzyl alcohol were added to the solution. This was followed by the dropwise addition of 2.4 g of pyridine and the mixture was stirred at room temperature overnight. The reaction mixture was then diluted with diethyl ether, washed with dilute aqueous hydrogen chloride and water, dried over anhydrous magnesium sulfate and distilled to remove the low-boiling fraction. The residual viscous oil was purified by column chromatography. By the above procedure there were obtained 3.9 g of 3-phenoxybenzyl β-(1,3,3-trichloroallyl)isovalerate (3-phenoxybenzyl 4,6,6-trichloro-3,3-dimethyl-5-hexenoate, Compound [17]) the NMR spectrum and elemental analysis of which are given below [yield: 91%].

Provenance & Evidence