反应详情

A solution of 30.0 g of 5-ethyl-salicylaldehyde (Reg.No. 52411-35-5) in 500 ml of DMF was treated with 36.0 g of sodium iodide and 67.6 g of Chloroamine T and stirred for one hour at room temperature. The reaction mixture was concentrated in a high vacuum, poured into ice-water, made acid with 2N hydrochloric acid and extracted with ethyl acetate. The organic phases were washed with aqueous sodium thiosulphate solution, saturated sodium chloride solution and ice-water, dried over sodium sulphate and concentrated. The residue was taken up in ether-hexane (1:1) and filtered. The filtrate was concentrated and gave 45.8 g of 5-ethyl-2-hydroxy-3-iodo-benzaldehyde; MS (EI) m/z 276 M+.

1. concentrationThe reaction mixture was concentrated in a high vacuum
2. additionpoured into ice-water
3. extractionextracted with ethyl acetate
4. washThe organic phases were washed with aqueous sodium thiosulphate solution, saturated sodium chloride solution and ice-water
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. filtrationfiltered
8. concentrationThe filtrate was concentrated