Lithium Hydroxide → HCID 44249133, compound

Participants

Reaction Steps

To a solution of the product from example 3 step e) (21.4 g) in THF (200 mL) was added a solution of lithium hydroxide (10.35 g) in water (40 mL) with vigorous stirring. After 45 min, aqueous 20% brine solution (160 mL) was added and the layers separated. The organic fraction was concentrated in vacuo, the residue re-dissolved in water (400 mL) and acidified to pH 2 with conc HCl whilst stirring. 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 at 40° C. to give the title product in crude form (˜20 g). A portion of this solid (1 g ) was recrystallised by heating to reflux in MeCN (5 mL) until dissolution, followed by cooling to RT, stirring for 16 h and collection of the resulting solid and drying in vacuo to afford the title product (0.759 g).

Provenance & Evidence