HRID653382

反应详情

EQUATION

反应方程式

HRID 653382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Octyloxy-4'-((S)-3-methyl-pentanoyl)biphenyl (24.6 g, 0.065 mol) obtained in Example 23 described later, 80% hydrazine hydrate (50 ml) and diethylene glycol (85 ml) were placed in a 500 ml three-neck flask, followed by heating with stirring, keeping the mixture at 120° C. for one hour, then cooling, adding, at a stroke, a solution of potassium hydroxide (8.8 g, 0.157 mol) in water (5 ml) while keeping the temperature at 50° C., distilling off so that the temperature of the system might become 200° C., reacting at 200° C. for 4 hours, then cooling, adding water (200 ml) and toluene (50 ml), transferring the contents into a separating funnel, water-washing the organic layer till the washing liquid became neutral, distilling off the solvent, distilling under reduced pressure to collect a fraction having a boiling point of 210°-213° C./3 mmHg, and recrystallizing it from ethyl alcohol (20 ml) and ethyl acetate (5 ml) to obtain 4-octyloxy-4'-((S)-3-methyl-pentyl)biphenyl (IIIb1) (13.5 g) which was a smectic liquid crystal exhibiting SC* phase and SH* phase, and whose phase transition points were as follows as shown in Table 2, column of Example 24: C-S1 point, 43.0° C.; Sl-SH* point, 57.9° C.; SH*-SC* point, 62.5° C; SC*-I point, 65.1° C.

WORKUP

后处理

  1. temperatureby heating
  2. customat 120° C.
  3. customfor one hour
  4. temperaturecooling
  5. additionadding, at a stroke
  6. customat 50° C.
  7. distillationdistilling off so that the temperature of the system
  8. custommight become 200° C.
  9. temperaturecooling
  10. additionadding water (200 ml) and toluene (50 ml)
  11. washwater-washing the organic layer till the washing liquid
  12. distillationdistilling off the solvent
  13. distillationdistilling under reduced pressure
  14. customto collect a fraction
  15. customrecrystallizing it from ethyl alcohol (20 ml) and ethyl acetate (5 ml)