HRID1742991
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 solution of compound of example K (1.0 g) in trifluoroacetic acid (4 ml) was stirred at room temperature under nitrogen for 10 minutes and concentrated. The residue was dissolved in methanol and treated with basic resin (ANGA-316) and filtered. The filtrate was concentrated and purified by column chromatography over neutral alumina using methanol/CHCl3 mixture as solvent. Yield 670 mg. 1H NMR (CD3OD) δ: 2.80 (m, 1H), 3.20-3.80 (m, 5H), 5.10 (m, 1H), 7.75 (s, 1H), 8.0 (S, 1H).
WORKUP
后处理
- concentrationconcentrated
- dissolutionThe residue was dissolved in methanol
- additiontreated with basic resin (ANGA-316) and
- filtrationfiltered
- concentrationThe filtrate was concentrated
- custompurified by column chromatography over neutral alumina