Lithium Hydroxide → HCID 6928767, compound

Participants

Reaction Steps

The product of formula (VIIa) (Intermediate 3, 18.0 g, 67.7 mmol) was dissolved in tetrahydrofuran (100 mL) and the resulting solution cooled to 5–10° C. A solution of lithium hydroxide (7 g) in water (140 mL) was added slowly, maintaining the reaction temperature to below 25° C. and the mixture was stirred for 24 hours at room temperature, then concentrated in vacuo until most of tetrahydrofuran had been removed. Concentrated HCl was added drop-wise to adjust the pH to 2, water (60 mL) was added and the slurry stirred at 0–10° C. for one hour. The precipitate was isolated by filtration, and dried in a vacuum oven. The crude product of formula (IIIa) was used without any further purification (9.35 g, 90%).

Provenance & Evidence