HRID431518

反应详情

EQUATION

反应方程式

HRID 431518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.38 g (0.7 mmol) of (2S)-2-(1-adamantylmethoxycarbonylamino)-3-((5-(2-(1,4,5,6-tetrahydropyrimidin-2-ylcarbamoyl)-ethyl)-thiophene-2-carbonyl)-amino)-propionic acid (example 15) were dissolved in 7 ml of isobutanol. Under an inert gas atmosphere and under external ice cooling 0.19 ml of thionyl chloride were cautiously added. After stirring for 8 hours at room temperature the reaction was complete. The solvents were removed in vacuo to give a colourless foam which was purified by chromatography (silica gel; isopropanol/ethyl acetate/water (4/3/1; v/v/v)). The fractions containing the title compound were lyosphilized to give 0.30 g of a colourless solid.

WORKUP

后处理

  1. customThe solvents were removed in vacuo
  2. customto give a colourless foam which
  3. customwas purified by chromatography (silica gel; isopropanol/ethyl acetate/water (4/3/1; v/v/v))
  4. additionThe fractions containing the title compound