HRID1654297

反应详情

EQUATION

反应方程式

HRID 1654297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of the product from Example 7, Step II (1.5 g, 0.00524 mol), the product from Step V above 1.45 g, 0.00576 mol), sodium bicarbonate (0.88 g, 0.0105 mol) and acetonitrile (45 ml) was warmed at 90°-95°, under nitrogen for 6 hours and kept at ambient temperature for 11 hours. It was then filtered. The filtrate was concentrated and the residue chromatographed on silica gel with 0.5% NH4OH-6% MeOH--CH2Cl2 to give 1.63 g of the titled compound which is a compound of Formula I'. The high resolution mass spectrum had m/z 456 (M+). Theory for C23H40N2O5S: 456.2658; measured: 456.2650.

WORKUP

后处理

  1. filtrationIt was then filtered
  2. concentrationThe filtrate was concentrated
  3. customthe residue chromatographed on silica gel with 0.5% NH4OH-6% MeOH