Lithium Hydroxide → HCID 44249133, compound

Participants

Reaction Steps

To a vigorously stirred slution of the product from step e) (307 g) in THF (3 L) was added a solution of lithium hydroxide (148 g) in water (0.6 L) and the reaction stirred at RT for 45 min. Aqueous 20% brine solution (2.5L) was added and the layers separated. The organic fraction was concentrated in vacuo, the residue re-dissolved in water (6 L) and the stirred mixture acidified to pH 1 with conc HCl. The resulting precipitate was filtered and washed with portions of water until the filtrate was pH 6. Iso-hexane was eluted through the filter cake to remove excess water and the solid was dried in a vacuum oven for 48 h at 40° C. to give the title product in crude form (259 g).

Provenance & Evidence