HRID1965164
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A 500 mL Parr bottle was charged with crude 16 (50 mg, 0.08 mmol) and 10% Pd-on-carbon (50 mg) in reagent grade MeOH (3 mL). The mixture was pressurized to 50 PSI H2 then shaken for 2 h. The catalyst was removed by filtration through Celite® and the solids were washed with MeOH and EtOAc. The filtrate was concentrated in vacuo. The crude product was purified by RP-HPLC (2″ Dynamax® C18, 10-70% ACN/water containing 0.1% HOAc over 30 min; Flow: 40 mL/min) to afford 20 mg (51%) of 17 after lyophilization.
WORKUP
后处理
- customThe catalyst was removed by filtration through Celite®
- washthe solids were washed with MeOH and EtOAc
- concentrationThe filtrate was concentrated in vacuo
- customThe crude product was purified by RP-HPLC (2″ Dynamax® C18, 10-70% ACN/water containing 0.1% HOAc over 30 min