HRID1486377

反应详情

EQUATION

反应方程式

HRID 1486377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of Compound 13 (1.00 g, 2.28 mmol), 2,2′-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3-phenylene)bis(benzo[d]oxazole) (1.159 g, 2.37 mmol), tetrakis(triphenylphosphine) palladium(0) (0.13 g, 0.11 mmol), potassium carbonate (0.95 g, 6.85 mmol), 1,4-dioxane (20.00 mL), and water (4.00 mL) was degassed with bubbling argon for 20 minutes at 45° C. The reaction was then heated to 100° C. and stirred overnight (16.5 hours), maintaining an argon atmosphere. The precipitated product was filtered, dried, and performed boiling ethyl acetate, chloroform, and methanol washes. The solid product was collected to yield Host-7 (0.75 g, 45%). 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 at 45° C
  2. temperaturemaintaining an argon atmosphere
  3. filtrationThe precipitated product was filtered
  4. customdried
  5. customThe solid product was collected
  6. customto yield Host-7 (0.75 g, 45%)