HRID555218

反应详情

EQUATION

反应方程式

HRID 555218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.5 g of bis[3-(carbazol-9-yl)phenyl]amine, 4.9 g of 9-(3-iodophenyl)carbazole, 2.1 g of sodium tert-butoxide, 0.1 g of palladium acetate, and 50 ml of anhydrous toluene were added in a flask under a nitrogen atmosphere. At an inner temperature of 71° C., 0.4 g of tert-butylphosphine was added by using a syringe. After 10 hours of reaction at 100° C., 300 ml of toluene was added to extract the objective substance, followed by filtration. The filtrate was concentrated to dryness to obtain a crude product. The dried crude product was purified by column chromatography to obtain 5.3 g (yield 56%) of mTCTA (Compound 2). The product was identified by 1H-NMR analysis (see FIG. 1). The following 36 hydrogen atoms were detected upon 1H-NMR (CDCl3) analysis. δ (ppm): 8.083-8.130 ppm (6H), 7.468-7.565 ppm (6H), 7.128-7.390 ppm (24H).

WORKUP

后处理

  1. customAfter 10 hours of reaction at 100° C.
  2. extractionto extract the objective substance
  3. filtrationfollowed by filtration
  4. concentrationThe filtrate was concentrated to dryness
  5. customto obtain a crude product
  6. customThe dried crude product
  7. customwas purified by column chromatography