反应详情

温度

60 °C

2 g of 1-bromo-3-methyl-butan-2-one obtained in step 93-1 was added to 20 ml of ethanol and 920 mg of thiourea was added thereto. The mixture was heated to 60° C., stirred for 3.5 hr and cooled to room temperature. The resulting mixture was added with aqueous sodium carbonate and extracted twice with ethyl acetate. The organic layer was washed with water and saline solution, dried over anhydrous magnesium sulfate and concentrated under a reduced pressure. The resulting residue thus obtained was purified by column chromatography (ethyl acetate/hexane=1/2) to obtain 1.2 g of the title compound.

1. additionwas added
2. temperaturecooled to room temperature
3. extractionextracted twice with ethyl acetate
4. washThe organic layer was washed with water and saline solution
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated under a reduced pressure
7. customThe resulting residue thus obtained
8. customwas purified by column chromatography (ethyl acetate/hexane=1/2)