反应详情

温度

150 °C

To 350 ml of xylene were added 341 g (1280 mmol) of the crude 3-(trans-4-(trans-4-propylcyclohexyl)cyclohexyl)propanol obtained by the procedures described above and 881 g (5120 mmol) of 47% hydrobromic acid, water was removed by azeotropic distillation, and then the mixture was stirred at 150° C. for 2 hours. To the reaction mixture was added 1.0 l of toluene, and it was washed with 300 ml of saturated aqueous sodium carbonate solution twice and with 400 ml of water thrice, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under a reduced pressure, and the residue was subjected to silica gel column chromatography (eluent: heptane) to obtain 156 g of a crude 1-bromo-3-(trans-4-(trans-4-propylcyclohexyl)cyclohexyl)propane.

1. customobtained by the procedures
2. customwas removed by azeotropic distillation
3. additionTo the reaction mixture was added 1.0 l of toluene, and it
4. washwas washed with 300 ml of saturated aqueous sodium carbonate solution twice
5. dry with materialwith 400 ml of water thrice, and then dried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under a reduced pressure