HRID719695

反应详情

EQUATION

反应方程式

HRID 719695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Prepared in the same manner as described for example 1. A solution of 4′-(2-phenoxy-ethylsulfanylmethyl)-biphenyl-2-carboxylic acid (0.38 g, 1.04 mmol, 1 eq.) in anhydrous THF was treated with 1,1′-carbonyldiimidazole (0.17 g, 1.06 mmol, 1.02 eq.) and warmed as described. The reaction was allowed to cool and then treated with 3-(dimethylamino)propylamine (0.13 g, 1.25 mmol, 1.2 eq.). The reaction was treated as described in example 1 to give a yellow oil. The oil was purified by silica gel flash chromatography using 10% 2M NH3 in methanol in diethyl ether as the mobile phase. Fractions containing the product were pooled and the solvent removed in vacuo leaving 4′-(2-phenoxy-ethylsulfanylmethyl)-biphenyl-2-carboxylic acid (3-dimethylamino-propyl)-amide (0.40 g, 85% yield) as a light yellow oil.

WORKUP

后处理

  1. customPrepared in the same manner
  2. temperaturewarmed
  3. temperatureto cool
  4. additionThe reaction was treated
  5. customto give a yellow oil
  6. customThe oil was purified by silica gel flash chromatography
  7. additionFractions containing the product
  8. customthe solvent removed in vacuo