HRID2262335

反应详情

EQUATION

反应方程式

HRID 2262335 的结构方程式

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

As shown in the following Reaction 9, 100 mg (0.42 mmol) of 2-(4-bromo-phenyl)-thiophene synthesized in C of Example 1-2 was melted in 5 mL of n-phentanol, and 130 mg (0.84 mmol, 2 eq) of sodium iodide and 0.004 mL (0.042 mmol, 10 mol %) of 1,3-diaminopropane was added thereto, and then the reaction solution was refluxed for 18 hours at temperature of 130° C. Next, the reaction solution was washed with aqueous ammonia, and was dehydrated with magnesium sulfate, filtered, and then distilled under reduced pressure. The compound distilled under reduced pressure was purified with a column chromatography (mobile phase: n-hexane) to obtain 100 mg of 2-(4-iodo-phenyl)-thiophene with the yield of 83.3%. NMR data of the obtained compound is as follows. [1H NMR (400 MHz, CDCl3): δ 7.52 (m, 4H), 7.33 (d, 2H), 7.10 (t, 1H)].

WORKUP

后处理

  1. customsynthesized in C of Example 1-2
  2. additionwas added
  3. washNext, the reaction solution was washed with aqueous ammonia
  4. filtrationfiltered
  5. distillationdistilled under reduced pressure
  6. distillationThe compound distilled under reduced pressure
  7. customwas purified with a column chromatography (mobile phase: n-hexane)