反应详情

To a suspension of 560.0 mg of compound (15) as obtained from example 9 (1.983 mmol) in 11.2 mL dimethoxyethane were added dropwise at 0° C. 1.68 mL concentrated aqueous hydrochloric acid (36.5%) (19.83 mmol, 10.0 eq). The ice bath was removed after 15 min and the triphasic mixture was vigorously stirred. After 4 h, the mixture was evaporated to dryness in a rotary evaporator (27° C., 5 mbar, then 1 mbar). The crude product was obtained as a lightly yellow semisolid (805.4mg, 194% by weight).333.3 mg crude product were purified by trituration with 0.7 mL methanol at room temperature for 18 h furnishing the title compound (168.7 mg, 0.425 mmol, 98% by weight) as white crystals.

1. additionwere added dropwise at 0° C
2. customThe ice bath was removed after 15 min
3. customthe mixture was evaporated to dryness in a rotary evaporator (27° C., 5 mbar
4. customThe crude product was obtained as a lightly yellow semisolid (805.4mg, 194% by weight)
5. custom333.3 mg crude product were purified by trituration with 0.7 mL methanol at room temperature for 18 h