HRID335355

反应详情

EQUATION

反应方程式

HRID 335355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

In a one-necked flask, tetradodecyl benzo[1,2-b:4,5-b′]dithiophene-4,4,8,8-tetracarboxylate (9.0 g, 8.65 mmol) was dispersed in DMF (80 mL). The mixture was stirred at 120° C. for 10 minutes until the solution became clear. After air was purged in the flask, NaI (800 mg) was added and the reaction mixture was refluxed for 24 hours. After the solvent was evaporated under vacuum, water (30 mL) was added to the residue to form a mixture, which was extracted with CH2Cl2. The organic layer was combined, dried, and concentrated. The crude product was purified by flash chromatography (eluent: CH2Cl2:hexane=7:3) to give didodecyl benzo[1,2-b:4,5-b′]dithiophene-4,8-dicarboxylate (yield: 1.75 g, 32.9%). 1H NMR (CDCl3): 0.9 (6H, t), 1.3 (28H, m), 1.4 (4H, m), 1.6 (4H, m), 1.9 (4H, m), 4.6 (4H, t), 7.8 (2H, d), 8.3 (2H, d).

WORKUP

后处理

  1. customAfter air was purged in the flask, NaI (800 mg)
  2. additionwas added
  3. temperaturethe reaction mixture was refluxed for 24 hours
  4. customAfter the solvent was evaporated under vacuum, water (30 mL)
  5. additionwas added to the residue
  6. customto form a mixture, which
  7. extractionwas extracted with CH2Cl2
  8. customdried
  9. concentrationconcentrated
  10. customThe crude product was purified by flash chromatography (eluent: CH2Cl2:hexane=7:3)