Lithium tri-tert-butoxyaluminohydride → HCID 20271480, compound

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Reaction Steps

Stir a mixture of the crude 8-nitrodibenzo[b,f]thiepin-3-carboxylic acid chloride in dry tetrahydrofuran at -78° C. under nitrogen, and add dropwise a filtered solution of 1.1 equivalents of lithium tri-tertiarybutoxy-aluminum hydride in tetrahydrofuran. Stir the mixture for 30 minutes at -78° C. and allow to warm to ambient temperature. Add the mixture to ice-cold dilute hydrochloric acid, and isolate the product by extraction with chloroform. Purify the title compound by chromatography on silica gel using a mixture of ethyl acetate and toluene for elution.

Provenance & Evidence