反应详情

Equimolar quantities of ethyl 2-acetyl-3-ethoxy-2-propenoate 1 (20.0 g, 107 mmol), ((amino(imino)methyl)-sulfanyl)methane 2 (9.68 g, 107 mmol) and triethylamine (10.8 g, 107 mmol) in EtOH (100 mL) were stirred at reflux for 48 hours. Then reaction mixture was concentrated and diluted with water. The biphasic mixture was transferred into a separatory funnel and extracted with DCM. Organic extract was washed with water, dried, filtered, and concentrated. The product was purified by crystallization from ethanol/water to yield in a colorless solid (18.4 g, 86.7 mmol, 81%).

1. temperatureat reflux for 48 hours
2. customThen reaction mixture
3. concentrationwas concentrated
4. additiondiluted with water
5. customThe biphasic mixture was transferred into a separatory funnel
6. extractionextracted with DCM
7. extractionOrganic extract
8. washwas washed with water
9. customdried
10. filtrationfiltered
11. concentrationconcentrated
12. customThe product was purified by crystallization from ethanol/water