反応 #1256741

反応方程式

ammonium chloride

n-pentane

Diisobutylchlorosilane

THF

→

tert-Butyldiisobutylsilane

反応条件

後処理

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

実験手順

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%).

出典