HRID1965177
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
The Cbz-protected intermediate 31 (180 mg, 0.27 mmol) was stirred vigorously with 10% Pd-on-carbon (wet, 100 mg, 0.09 mmol) in MeOH (20 mL) under 1 atm H2. After 4 h, the catalyst was removed by filtration with an Acrodisc® 0.45 μm nylon membrane syringe filter and the solvent was removed in vacuo. The crude product was purified by reverse-phase HPLC (2″ Dynamax® C18, 10-55% ACN/water containing 0.1% HOAc over 20 min; Flow: 40 mL/min) to afford 45 mg of 32 (32%, 3 steps) as a flocculent, white solid following lyophilization.
WORKUP
后处理
- customthe catalyst was removed by filtration with an Acrodisc® 0.45 μm nylon membrane syringe
- filtrationfilter
- customthe solvent was removed in vacuo
- customThe crude product was purified by reverse-phase HPLC (2″ Dynamax® C18, 10-55% ACN/water containing 0.1% HOAc over 20 min