反应详情

A solution of vinylbromide (11.8 g, 110 mmol) in 40 ml tetrahydrofuran was added to a mixture of magnesium (2.79 g, 115 mmol) in 20 ml tetrahydrofuran under a nitrogen atmosphere at 50° to 60° C. After reflux for 1 h 3-(4-chlorobenzoyl)pyridine (21.8 g, 0.100 mol) in 100 ml tetrahydrofuran was added at 10° C. After stirring for 1 h a solution of 8 g ammonium chloride in 40 ml water was added and the mixture filtrated. The organic phase was dried over sodium sulphate and evaporated to give 29.4 g of a red oil containing 20% unreacted starting ketone. This crude product was used directly in the next step (Example C).

1. additionwas added at 10° C
2. additionwas added
3. filtrationthe mixture filtrated
4. dry with materialThe organic phase was dried over sodium sulphate
5. customevaporated