HRID901210
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 suspension of 1B (1 g, 2.33 mmol) and platinium 5% wt on activated carbon (600 mg) in THF (30 mL) and MeOH (30 mL) was stirred at RT under H2 at 75 psi for 2 days. The reaction mixture was filtered and the filtrate was concentrated. The residue was purified by silica gel (40 g) column chromatography eluting with a gradient of methanol (0-6%) in EtOAc/hexane (1:1) to give the title compound as a white foam (360 mg, 36%). LC/MS (method A): retention time=2.77 min, (M+H)+=430.
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated
- customThe residue was purified by silica gel (40 g) column chromatography
- washeluting with a gradient of methanol (0-6%) in EtOAc/hexane (1:1)