HRID1486381

反应详情

EQUATION

反应方程式

HRID 1486381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of Compound 17 (1.25 g, 2.56 mmol), 2,2′-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3-phenylene)bis(benzo[d]oxazole) (1.23 g, 2.82 mmol), tetrakis(triphenylphosphine) palladium(0) (0.15 g, 0.13 mmol), potassium carbonate (1.06 g, 7.68 mmol), 1,4-dioxane (35.00 mL), and water (7.00 mL) was degassed with bubbling argon for 20 minutes. The reaction was then heated to 100° C. and stirred overnight (16.5 hours), maintaining an argon atmosphere. After adding water, the precipitated product was filtered, dried, washed with dichloromethane, and recrystallized from chloroform/acetone. The recrystallized product was collected to yield Host-11 (1.13 g, 61%). Confirmed by LCMS (APCI): calculated for C50H29N3O3 (M+H): 720. Found: 720.

WORKUP

后处理

  1. customwas degassed with bubbling argon for 20 minutes
  2. temperaturemaintaining an argon atmosphere
  3. additionAfter adding water
  4. filtrationthe precipitated product was filtered
  5. customdried
  6. washwashed with dichloromethane
  7. customrecrystallized from chloroform/acetone
  8. customThe recrystallized product was collected
  9. customto yield Host-11 (1.13 g, 61%)