反应 #66036

反应方程式

acetyl chloride

AlCl3

1-(4-carbazol-9-yl-phenyl)-ethanone

p-fluorobenzoyl chloride

AlCl3

→

1-{4-[3-Acetyl-6-(4-fluoro-benzoyl)-carbazol-9-yl]-phenyl}-ethanone

溶剂

CH2Cl2

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature overnight
2. 2
   萃取the crude product is extracted twice with CH2Cl2
3. 3
   洗涤The combined organic layer is washed with H2O and brine
4. 4
   干燥dried over MgSO4
5. 5
   浓缩concentrated
6. 6
   其他to give the residue, which
7. 7
   其他is purified
8. 8
   洗涤by washing with hot TBME (tert-butyl methyl-ether)
9. 9
   其他The structure of the product, which is obtained as a white solid

实验过程

To 1-(4-carbazol-9-yl-phenyl)-ethanone (5.71 g) in CH2Cl2 (150 mL) is added p-fluorobenzoyl chloride (3.17 g) and AlCl3 (5.41 g) at 0° C. After stirring overnight at room temperature, acetyl chloride (1.73 g) and AlCl3 (2.93 g) are further added at 0° C. and the mixture is stirred at room temperature overnight. The reaction mixture is poured into ice-water, and the crude product is extracted twice with CH2Cl2. The combined organic layer is washed with H2O and brine, dried over MgSO4, and concentrated to give the residue, which is purified by washing with hot TBME (tert-butyl methyl-ether). The structure of the product, which is obtained as a white solid, is confirmed by the 1H-NMR spectrum (CDCl3). δ [ppm]: 2.73 (s, 3H), 2.75 (s, 3H), 7.23 (t, 2H), 7.48 (d, 1H), 7.51 (d, 1H), 7.72 (d, 2H), 7.91 (dd, 2H), 7.99 (d, 1H), 8.14 (d, 1H), 8.28 (d, 2H), 8.66 (s, 1H), 8.80 (s, 1H).

来源