Реакция #1256741
ord-ec5fb26113ea454f83377c8a91b4bf8d
Реактанты
Реагенты
Условия реакции
Обработка
- 1workup.WAITThe reaction mixture was left
- 2Температураto cool
- 3ПромывкаThe formed organic layer was washed three times with water
- 4Сушкаonce with saturated brine, and the thus-washed layer was dried over sodium sulfate anhydrate
- 5ДругоеThe solvent was removed
- 6workup.DISTILLATIONfollowed by purification through distillation under reduced pressure, whereby the Compound 36a
- 7Другоеwas obtained as a colorless liquid (boiling point; 27 mmHg, 100° C. fraction, 13.6 g, 68%)
Методика
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%).