HRID617679
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 217.5 °C
PROCEDURE
实验过程
Phthalonitrile (1100 grams) and titanium tetrachloride (813 grams) were suspended in 6800 milliliters (ml) of 1-chloronaphthalene and heated to 215-220° C. and maintained for 2.5 hours at this temperature. The reaction mixture was cooled to 140° C., and the dark solid was collected and washed with acetone and methanol. After drying, the dark blue solid (1090 grams) was slurried twice in refluxing 10 liters of distilled water for two hours, filtered hot each time, and washed with acetone to yield crude phthalocyanine. The X-ray diffraction spectrum exhibits major peaks of the Bragg angle at 7.5, 8.3, 10.5, 12.7, 14.2, 14.6, 18.9, 22.1, 24.3, 26.1, and 29.9 (all ±0.2 degrees).
WORKUP
后处理
- temperaturemaintained for 2.5 hours at this temperature
- temperatureThe reaction mixture was cooled to 140° C.
- customthe dark solid was collected
- washwashed with acetone and methanol
- customAfter drying
- temperaturein refluxing 10 liters of distilled water for two hours
- filtrationfiltered hot each time
- washwashed with acetone