反应详情

20 g of methoxythioacetamide are added, with vigorous stirring, to 31.3 g of 2-chloroacetoacetic acid ethyl ester in 400 ml of benzene at room temperature and then, using a water separator, heated under reflux for 41/2 hours. After cooling to room temperature, the benzenic reaction solution is diluted with 500 ml of ethyl acetate, washed twice using 80 ml of 10% sodium carbonate solution each time and twice using 50 ml of water each time, dried over sodium sulfate and filtered. The solvent mixture is evaporated off. The yellow oil that remains is crystallised by trituration with diisopropyl ether. The beige-coloured crystals melt at 36°-37° C.

1. temperatureheated
2. temperatureunder reflux for 41/2 hours
3. washwashed twice
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customThe solvent mixture is evaporated off
7. customThe yellow oil that remains is crystallised by trituration with diisopropyl ether
8. custommelt at 36°-37° C.