HRID65171

反应详情

EQUATION

反应方程式

HRID 65171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.20 g of 4-(trans-4-pentylcyclohexyl)-4'-[2-(trans-4-pentylcyclohexyl)vinyl]biphenyl were suspended in toluene/ethanol (3:2) in a sulphonation flask, treated with 200 mg of palladium/carbon (10%) and hydrogenated at normal pressure and 50° C. until the hydrogen uptake came to a standstill. Filtration of the mixture and concentration of the filtrate gave a white semi-crystalline residue which, after recrystallization from 100 ml of hexane, yielded 1.55 g of 4-(trans-4-pentylcyclohexyl)-4'-[2-(trans-4-pentylcyclohexyl)ethyl]biphenyl as colourless needles; transition (presumably S-S) 219.5° C., transition S-N 243.2° C., cl.p. (N-I) 256.1° C. This substance was found to be very strongly super-coolable; upon cooling to room temperature it still did not crystallize. Rf-value (hexane): 0.32.

WORKUP

后处理

  1. filtrationFiltration of the mixture and concentration of the filtrate
  2. customgave a white semi-crystalline residue which
  3. customafter recrystallization from 100 ml of hexane