HRID262413

反应详情

EQUATION

反应方程式

HRID 262413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a round-bottomed flask fitted with thermometer, reflux condenser and stirrer is placed a mixture of 25 ml. glacial acetic acid and 50 ml methanol and in it is dissolved 2.38 g (0.1 mol) 1,4-diaminoanthraquinone. There is then added 4.68 g (0.2 mol) p-octyloxybenzaldehyde and the mixture is heated at 90° for one hour. The reaction mixture is cooled to about 20°-25° and poured into ice water. The precipitated product is collected and recrystallized from ethylene glycol monomethyl ether or 1:1 methanol water as small purple needles. The crystallization is repeated twice more to obtain 1,4-bis(p-octyloxybenzylidene amino)anthraquinone m.b. 280° (dec) having absorption spectra in visual and infra red ranges as shown in FIGS. 9, 10 and 11 and of sufficient purity for use in guest-host combinations. Analysis: Calculated for C44H54N2O4 ; 78.3%C, 8.06%H, 4.15%N: found 77.61%C, 7.46%H, 4.18%N.

WORKUP

后处理

  1. customIn a round-bottomed flask fitted with thermometer
  2. temperaturereflux condenser and stirrer
  3. additiona mixture of 25 ml
  4. temperaturethe mixture is heated at 90° for one hour
  5. temperatureThe reaction mixture is cooled to about 20°-25°
  6. customThe precipitated product is collected
  7. customrecrystallized from ethylene glycol monomethyl ether or 1:1 methanol water as small purple needles
  8. customThe crystallization