HRID1742991

反应详情

EQUATION

反应方程式

HRID 1742991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in methanol
  3. additiontreated with basic resin (ANGA-316) and
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. custompurified by column chromatography over neutral alumina