HCID 178496632、化合物 → Sirolimus

関与物質

反応条件

反応手順

Crude CCI-779 boronate (300 g) and acetone (900 g) was charged into a flask. The mixture was heated to reflux (55 to 61° C.) and held for 1 h. The mixture was cooled to 20-25° C. over 2-3 h, then distilled to remove acetone under vacuum (23-26″ Hg) at a pot temperature not exceeding 10-18° C. (final volume 940-960 mL). The diethyl ether (450 g) was added, stirred at 18-25° C. for 18 hours, and then filtered to give crude CCI-779 boronate (225 g, LOD=0.95%). The filtered crude CCI-779 boronate (224 g) and acetone (676 g) was charged into a flask. The mixture was heated to reflux (55 to 61° C.) and held for 1 h. The mixture was cooled to 19-25° C. over 2-3 h, then distilled to remove acetone under vacuum (18-20″ Hg) at a pot temperature of 18-20° C. (final volume 620 mL). The diethyl ether (338 g) was added, stirred at 18-25° C. for 18 hours, and then filtered. After washing 3 times using ether (250 mL each) to give CCI-779 boronate in 63% yield (LOD=0.57%, strength=85.9%, total impurities=1.8%, LSI=0.50, rapamycin=0.95%).

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