反应详情

温度

60 °C

A solution of p-(trans-4-hexylcyclohexylcarbonyloxy)-benzoyl chloride (3.9 g) dissolved in toluene was added to a solution of 5-hexylpyrimidin-2-ol (1.0 g) in pyridine (10 ml), followed by stirring at 60° C. for 2 hours, allowing the mixture to stand at room temperature overnight, adding water and toluene to the reaction mixture, separating the toluene layer containing the reaction product, washing the toluene solution twice with 6NHCl (30 ml), washing with water, washing 5 times with 2N NaOH (100 ml), finally washing with water till the washing water became neutral, drying the resulting toluene solution, distilling off low boiling mixture of solvent, etc. under reduced pressure, and recrystallizing crystals obtained from the residue from n-heptanol solvent to obtain the objective compound (2.0 g) (yield 73%), which had a C-N point of 53.3° C. and a N-I point of 125.3° C.

1. waitto stand at room temperature overnight
2. customseparating the toluene layer
3. additioncontaining the reaction product
4. washwashing the toluene solution twice with 6NHCl (30 ml)
5. washwashing with water
6. washwashing 5 times with 2N NaOH (100 ml)
7. washfinally washing with water till the washing water
8. dry with materialdrying the resulting toluene solution
9. distillationdistilling off low
10. additionmixture of solvent, etc. under reduced pressure
11. customrecrystallizing crystals
12. customobtained from the residue from n-heptanol solvent