Ammonia → HCID 117651054, compound

Participants

Reaction Steps

Finely crushed 1 (140 mg, 0.330 mmol) was suspended in a mixed solvent of 1,4-dioxane (31.5 ml), THF (31.5 ml), and Et2O (7.0 ml), and the resultant mixture was irradiated with ultrasonic waves for 15 seconds. The mixture was further charged with 28% aq. NH3 (2.8 ml), and irradiated with ultrasonic waves for 15 seconds. The mixture was vigorously stirred for 14 hours at room temperature, and then left to stand for 1 hour at 5° C. The reaction mixture was then filtered using a membrane filter (H010A047A, Advantec). The filtered product was successively washed with water, THF, and Et2O, and dried under reduced pressure to obtain the target product Compound 1-NH4+ (134 mg, 92%) as a dark red solid.

Provenance & Evidence