HRID2221083

反应详情

EQUATION

反应方程式

HRID 2221083 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 2′,3′,5′-tri-O-acetyl-formycin A (prepared from formycin A by modification of the method from Synthesis (1989) 401) (1.1 g, 2.8 mmol) and n-butyl nitrite (2.6 ml, 22 mmol) in THF (30 ml) was heated at 50° C. for 25 h. After cooling to room temperature, the solvent was removed under reduced pressure. The mixture was dissolved in EtOH and reconcentrated (in each case twice). Silica gel chromatography using 2% MeOH in DCM gave compound (Ia) (0.49 g, 46%), the analysis of which confirmed the chemical identity with the product from method A.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. customthe solvent was removed under reduced pressure
  3. dissolutionThe mixture was dissolved in EtOH
  4. customgave compound (Ia) (0.49 g, 46%)