HRID537591

反应详情

EQUATION

反应方程式

HRID 537591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

5.4 g (21.1 mmol) of 9-bromoanthracene, 2.6 g (21.1 mmol) of phenylboronic acid, 60 mg (0.21 mmol) of palladium(II) acetate (abbreviation: Pd(OAc)2), 10 mL (20 mmol) of a potassium carbonate aqueous solution (2 mol/L), 263 mg (0.84 mmol) of tris(ortho-tolyl)phosphine (abbreviation: P(o-tolyl)3), and 20 mL of 1,2-dimethoxyethane (abbreviation: DME) were put in a 200 mL three neck flask, and then stirred for nine hours at 80° C. in nitrogen stream. After reaction, a precipitated solid was collected by suction filtration. Subsequently, the solid was dissolved in toluene and then filtered through florisil, celite, and alumina. After a filtrate was washed with water and saturated saline, it was dried with magnesium sulfate. After the mixture was subjected to natural filtration, when the filtrate was concentrated, 21.5 g of 9-phenylanthracene which was a target substance was obtained as a light brown solid at a yield of 85% (Synthesis scheme (b-1)).

WORKUP

后处理

  1. customAfter reaction
  2. filtrationa precipitated solid was collected by suction filtration
  3. dissolutionSubsequently, the solid was dissolved in toluene
  4. filtrationfiltered through florisil, celite, and alumina
  5. washAfter a filtrate was washed with water and saturated saline, it
  6. dry with materialwas dried with magnesium sulfate
  7. filtrationAfter the mixture was subjected to natural filtration, when the filtrate
  8. concentrationwas concentrated
  9. customwas obtained as a light brown solid at a yield of 85% (Synthesis scheme (b-1))