反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
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
- stirringthe resulting mixture was stirred for 15 minutes
- temperatureThe temperature of the mixture was increased to 150° C.
- temperaturethis temperature was maintained for 2 hours
- stirringThe mixture was stirred
- temperatureto cool down to a room temperature
- customThe resulting reaction mixture
- filtrationThen it was filtered
- customdried in an oven for 1 day
- customThe solid was crystallized from dimethylformamide (200 cm3)
- filtrationThe final filtered product
- washwas rinsed with methanol (100 cm3)
- customdried in a 100° C. vacuum oven