HRID890902

反应详情

EQUATION

反应方程式

HRID 890902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

4-Hydroxy-4′-cyanobiphenyl (10.35 g, 53.0 mmol), 6-chloro-1-hexanol (9.05 g, 66.3 mmol), cesium carbonate (18.99 g, 58.3 mmol), and potassium iodide (0.88 g, 5.3 mmol) were dissolved in N,N-dimethylformamide (DMF, 130 mL). The reaction mixture was stirred at 80° C. for 6 h. The resultant salt was removed by hot filtration. The filtrate was slowly added to 600 mL water, and the crude product was collected for recrystallization from methanol to yield 8 (14.24 g, 91.0%). 1H NMR spectral data (400 MHz, CDCl3): δ 1.40-1.70 (m, 6H, CH2—), δ 1.87 (m, 2H, —CH2—), δ 3.69 (t, 2H, —CH2OAr), δ 4.03 (t, 2H, HOCH2—), δ 6.80–7.90 (m, 8H, aromatic rings).

WORKUP

后处理

  1. customThe resultant salt was removed by hot filtration
  2. additionThe filtrate was slowly added to 600 mL water
  3. customthe crude product was collected for recrystallization from methanol