HRID446985
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 mixture of 48 (450 mg, 0.63 mmol) and 10% palladium-on-carbon (wet, 90 mg) in MeOH (15 mL) was shaken at 50 psi under a H2 atmosphere. After 1.5 h, the mixture was filtered through a 0.45 μM filtering disc, washed with MeOH and concentrated. Purification by reverse-phase HPLC (2″ Dynamax® C18, 10-70% ACN in H2O with 0.1% HOAc over 30 min) afforded 49 (123 mg) as a white flocculent solid following lyophilization of the purified fractions.
WORKUP
后处理
- filtrationthe mixture was filtered through a 0.45 μM
- filtrationfiltering disc
- washwashed with MeOH
- concentrationconcentrated
- customPurification by reverse-phase HPLC (2″ Dynamax® C18, 10-70% ACN in H2O with 0.1% HOAc over 30 min)