HRID1686160

反应详情

EQUATION

反应方程式

HRID 1686160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

1-Benzyl-2,3-dimethyl-3-(4-sulphobutyl)-3H-indolium-5-sulphonate salt (2 g), 1-(5-carboxypentyl)-2,3-dimethyl-3-(4-sulphobutyl)-3H-indolium-5-sulphonate (2 g) and malonaldehyde bis-phenylimine (2 g) were dissolved in acetic acid: pyridine: acetic anhydride (4.5:4.5:1) (100 ml). The mixture was heated at 90° C. for 2 hours. The mixture went blue/green immediately. A small sample was diluted in water for UV measurement. UV/Vis absorption spectroscopy observed a peak at 650 nm showing formation of Cy5. The reaction mixture was stored overnight at +2° C. The mixture was rotary evaporated to yield an oil. This was pumped under vacuum for several hours to ensure dryness. The sticky solid was washed with acetonitrile (4×500 ml) to yield a dry powder that was filtered and washed with more acetonitrile. The solid was dried under vacuum. Yield: 3.05 g.

WORKUP

后处理

  1. customUV/Vis absorption spectroscopy
  2. customThe mixture was rotary evaporated
  3. customto yield an oil
  4. waitThis was pumped under vacuum for several hours
  5. washThe sticky solid was washed with acetonitrile (4×500 ml)
  6. customto yield a dry powder that
  7. filtrationwas filtered
  8. washwashed with more acetonitrile
  9. customThe solid was dried under vacuum