HRID1009768

反应详情

EQUATION

反应方程式

HRID 1009768 的结构方程式

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Synthesis of 2-(2-(benzo[d]oxazole-2-yl)naphthalene-6-yl)benzo[d]oxazole polyphosphoric acid (125 cm3) was heated at 70° C. for 1 hour while agitating. 0.1 mol of naphthalene-2,6-dicarboxylic acid was added and the resulting mixture was stirred for 15 minutes. 0.2 mol of 2-aminophenol was added in a dropwise fashion for 10 minutes. The temperature of the mixture was increased to 150° C. and then this temperature was maintained for 2 hours. The mixture was stirred to cool down to a room temperature. The resulting reaction mixture was stirred for 1 hour with ice water (1.5 dm3), and neutralized with a diluted sodium carbonate hydrate solution. Then it was filtered and dried in an oven for 1 day. The solid was crystallized from dimethylformamide (200 cm3). The final filtered product was rinsed with methanol (100 cm3) and then dried in a 100° C. vacuum oven. As a result, colorless needle-shaped crystalline 2-(2-(benzo[d]oxazole-2-yl)naphthalene-6-yl) benzo[d]oxazole was produced at a yield of 75%.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred for 15 minutes
  2. temperatureThe temperature of the mixture was increased to 150° C.
  3. temperaturethis temperature was maintained for 2 hours
  4. stirringThe mixture was stirred
  5. temperatureto cool down to a room temperature
  6. customThe resulting reaction mixture
  7. filtrationThen it was filtered
  8. customdried in an oven for 1 day
  9. customThe solid was crystallized from dimethylformamide (200 cm3)
  10. filtrationThe final filtered product
  11. washwas rinsed with methanol (100 cm3)
  12. customdried in a 100° C. vacuum oven