反应 #1256741

反应方程式

ammonium chloride

n-pentane

Diisobutylchlorosilane

THF

→

tert-Butyldiisobutylsilane

反应条件

后处理

1. 1
   workup.WAITThe reaction mixture was left
2. 2
   温度to cool
3. 3
   洗涤The formed organic layer was washed three times with water
4. 4
   干燥once with saturated brine, and the thus-washed layer was dried over sodium sulfate anhydrate
5. 5
   其他The solvent was removed
6. 6
   workup.DISTILLATIONfollowed by purification through distillation under reduced pressure, whereby the Compound 36a
7. 7
   其他was obtained as a colorless liquid (boiling point; 27 mmHg, 100° C. fraction, 13.6 g, 68%)

实验过程

Diisobutylchlorosilane (18.0 mL, 100 mmol) was dissolved in THF (100 mL), and tert-butyl magnesium chloride THF solution (10M, 100 mL) was added dropwise thereto under nitrogen for 30 minutes. Cuprous bromide (286 mg, 2.00 mmol) was added to the resultant mixture, followed by stirring at 70° C. for 8 hours. The reaction mixture was left to cool, and saturated aqueous ammonium chloride and n-pentane were added thereto. The formed organic layer was washed three times with water and once with saturated brine, and the thus-washed layer was dried over sodium sulfate anhydrate. The solvent was removed, followed by purification through distillation under reduced pressure, whereby the Compound 36a was obtained as a colorless liquid (boiling point; 27 mmHg, 100° C. fraction, 13.6 g, 68%).

来源