反应详情

温度

45 °C

A 12 L 3-necked round bottom flask was charged with 169.74 gm of the product of Example 111-12 and 3.5 L of methanol, warmed to 45° C., water (1.75 L) was slowly added, stirred at 45-48° C. for about 1 hour, and cooled to ambient temperature overnight. The slurry was filtered and washed with 2:1 methanol:water, suction dried for 1 hour and dried at 50° C. vacuum oven overnight to give 60.4 gm of the title compound (28:1 diastereomeric ratio as determined by HPLC (Column: XDB C8 15 cm, Eluent: CH3CN/10 mM Na2HPO4 with H3PO4 adjusted to pH 7, Gradient: 10% CH3CN to 90% CH3CN in 15 min, then hold for 10 min, column oven temperature: 35° C.).

1. temperaturecooled to ambient temperature overnight
2. filtrationThe slurry was filtered
3. washwashed with 2:1 methanol
4. dry with materialwater, suction dried for 1 hour
5. customdried at 50° C. vacuum oven overnight