反应详情

温度

-10 °C

Aluminium chloride (4.80 g, 32.0 mmol, 1.0 eq.) and 1-phenyloctane (6.84 g, 32.0 mmol) were dissolved in dry dichloromethane (10 mL) and cooled to −10° C. A solution of bromoacetyl bromide (3.14 mL, 32.0 mmol, 1.0 eq.) in dichloromethane (12 mL) was added dropwise and the mixture was allowed to return to r.t. while stirring overnight. The mixture was slowly poured into ice water (100 mL) and the aqueous phase was extracted with dichloromethane (3×50 mL). The combined organic layers were dried over MgSO4 and concentrated under reduced pressure. The product was obtained as brown, highly viscous oil and was used in the next reaction without purification. Yield: 8.90 g (62%), purity: 69% (GC).

1. customto return to r.t.
2. extractionthe aqueous phase was extracted with dichloromethane (3×50 mL)
3. dry with materialThe combined organic layers were dried over MgSO4
4. concentrationconcentrated under reduced pressure
5. customThe product was obtained as brown, highly viscous oil
6. customwas used in the next reaction without purification