反应详情

温度

70 °C

A mixture of 1.91 g (8.55.10−3 mol) of 4-bromophenylhydrazine hydrochloride and 0.73 g (8.9.10−3 mol) of sodium acetate in 17 ml of water is prepared and 2.05 ml (35.8.10−3 mol) of acetic acid are added. This mixture is subsequently heated to 70° C., with stirring, and a suspension of 2.0 g (8.54.10−3 mol) of ethyl ε-oxobenzenehexanoate in 27 ml of water is then added slowly. The reaction mixture is stirred at 70-80° C. for 45 min and then at room temperature for 12 hours, after which it is extracted with 2 times 50 ml of ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate and concentrated under reduced pressure to give 3.38 g of the expected compound, which is used directly in the next step.

1. customis prepared
2. additionis then added slowly
3. stirringThe reaction mixture is stirred at 70-80° C. for 45 min
4. extractionafter which it is extracted with 2 times 50 ml of ethyl acetate
5. washThe organic phase is washed with water
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under reduced pressure