تفاعل #66036

معادلة التفاعل

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

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature overnight
2. 2
   استخلاصthe crude product is extracted twice with CH2Cl2
3. 3
   غسيلThe combined organic layer is washed with H2O and brine
4. 4
   تجفيفdried over MgSO4
5. 5
   تركيزconcentrated
6. 6
   أخرىto give the residue, which
7. 7
   أخرىis purified
8. 8
   غسيلby washing with hot TBME (tert-butyl methyl-ether)
9. 9
   أخرىThe structure of the product, which is obtained as a white solid

الإجراء التجريبي

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).

المصدر