HRID976039

反应详情

EQUATION

反应方程式

HRID 976039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 4.24 g (7.6 mmol) of methyl bis-(1-naphthylmethyl)acetyl-(α-methyl-D-tryptophan) in 50 mL MeOH and 50 mL dioxane was treated with a solution of 1.0 g (25 mmol) of NaOH in 10 mL H2O and the solution left stirring at room temperature for 4 days. The solvent was removed under reduced pressure and the residue mixed with H2O and acidified to Congo red end point with dilute HCl. The crude product was collected and chromatographed on silica gel, eluting with CHCl3 : MeOH (95:5). There was obtained 2.37 g (57.8% yield) of the product as a solid foam. The structure was confirmed by NMR and mass spectroscopy.

WORKUP

后处理

  1. waitthe solution left
  2. customThe solvent was removed under reduced pressure
  3. additionthe residue mixed with H2O
  4. customThe crude product was collected
  5. customchromatographed on silica gel
  6. washeluting with CHCl3 : MeOH (95:5)