反応 #2678
ord-b0a83914dba048c6a657be3218f2bd5a
反応方程式
反応条件
後処理
- 1洗浄The product mixture is then washed with 1 liter of a 10% sodium carbonate solution
- 2乾燥The organic layer is dried with magnesium sulfate
- 3その他the methylene chloride is evaporated off
- 4温度to warm to room temperature
- 5その他The mixture is slowly quenched with 50 ml of water
- 6洗浄by washing with 1 liter of a 10% HCl solution
- 7乾燥The organic layer is dried with magnesium sulfate
- 8その他the solvent is evaporated
実験手順
This compound may be prepared in the following manner. Three moles of 1-bromooctane are slowly added to 3 moles of magnesium turnings in 0.6 liters of anhydrous ethyl ether (nitrogen atmosphere). One mole of diethyl carbonate in 0.151 anhydrous ethyl ether is slowly added to the mixture. The mixture is stirred for one hour at 30° C., then the mixture is slowly poured into 1.8 liters of a cold 10% HCl solution. The organic layer is dried with magnesium sulfate and the ethyl ether is evaporated off to give tri-n-octylcarbinol. One mole of tri-n-octylcarbinol is added to a mixture of 0.2 liters of methylene chloride and 0.32 moles calcium chloride. Approximately 1.5 moles of HCl gas is slowly bubbled through the solution. The product mixture is then washed with 1 liter of a 10% sodium carbonate solution. The organic layer is dried with magnesium sulfate and the methylene chloride is evaporated off. One mole of tri-n-octylmethylchloride is added to 0.75 liters of methylene chloride and the solution is blanketed with nitrogen and is cooled to 0° C. 0.33 moles of trimethylaluminum is then added and the mixture is allowed to warm to room temperature. The mixture is slowly quenched with 50 ml of water followed by washing with 1 liter of a 10% HCl solution. The organic layer is dried with magnesium sulfate and the solvent is evaporated to give tri-n-octylmethylmethane.