反应详情

The product from step 1 (4.8 g), thiourea (2.53 g) and potassium methylate (2.33 g) were heated together in boiling propan-2-ol (30 cm3) for 6 hours. The reaction mixture was allowed to cool overnight. The solvent was removed by evaporation under reduced pressure, the residue was dissolved in water and washed with ethyl acetate, the organic layer being discarded. The basic aqueous layer was acidified to pH 5 using glacial acetic acid and the product was extracted into ethyl acetate. Evaporation of the ethyl acetate under reduced pressure gave 3.769 g of an orange oil. 1H NMR (DMSO): δ3.46(6H,s); 5.14(1H,s); 6.94(1H,d); 7.18(1H,br s); 8.18(1H,d).

1. customfor 6 hours
2. temperatureto cool overnight
3. customThe solvent was removed by evaporation under reduced pressure
4. dissolutionthe residue was dissolved in water
5. washwashed with ethyl acetate
6. extractionthe product was extracted into ethyl acetate
7. customEvaporation of the ethyl acetate under reduced pressure