反应详情

33% hydrogen bromide in glacial acetic acid (20.7 ml) was added to a suspension of the product from stage 2 (4.14 g, 9.27 mmol) in glacial acetic acid (20.7 ml) and the mixture was stirred at room temperature for 1 h. The mixture was poured into diethyl ether (500 ml). The hydrobromide which had precipitated out was filtered off with suction, washed with diethyl ether and dried over potassium hydroxide in a desiccator. Saturated potassium carbonate solution (100 ml) was added to the salt (3.60 g) and the resulting mixture was extracted with methylene chloride (3×25 ml). The combined organic phases were dried with sodium sulfate and concentrated i. vac.

1. customThe hydrobromide which had precipitated out
2. filtrationwas filtered off with suction
3. washwashed with diethyl ether
4. dry with materialdried over potassium hydroxide in a desiccator
5. additionSaturated potassium carbonate solution (100 ml) was added to the salt (3.60 g)
6. extractionthe resulting mixture was extracted with methylene chloride (3×25 ml)
7. dry with materialThe combined organic phases were dried with sodium sulfate
8. concentrationconcentrated i