Water → HCID 77230206, compound

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Reaction Steps

Under a nitrogen atmosphere, 6.3 g of LiAlH4 (0.167 moles) are suspended in 250 mL of anhydrous diethyl ether and the temperature is reduced to 0° C. 43 g of (1b) (0.162 moles) in 75 mL of anhydrous diethyl ether are added dropwise and the mixture is stirred for 20 h. LiAlH4 is hydrolysed with water and 30% NaOH and the phases are separated. The aqueous phase is extracted repeatedly with diethyl ether, the organic phase is extracted with 1N HCl, the aqueous phase is alkalised with 30% NaOH, extracted with diethyl ether, the combined organic phases are washed to neutrality, dried with Na2SO4 and evaporated. 20.8 g of product are obtained, which are used in the subsequent step without further purification. Formula: C12H23NO (m.w. 197.32). Yield 65%.

Provenance & Evidence