反应详情

2-Nitromethylene-thiazolidine (7.3 g, 50 mmol) and 2-methyl-malonic acid bis-(2,4,6-trichloro-phenyl) ester (23.8 g, 50 mmol) in xylene (80 mL) was taken in a reaction flask and the flask was heated to reflux for 3 hours. The reaction mixture was monitored by TLC (100% ethylacetate). The reaction mixture was cooled, concentrated and partitioned between DCM and water. The organic layer was washed with water, brine solution, dried over Na2SO4 and concentrated. The crude product was kept at 0° C. for overnight. The solid formed was collected and washed with hexane and ether to afford 5.3 g of the product (46% yield).

1. temperaturethe flask was heated
2. temperatureto reflux for 3 hours
3. temperatureThe reaction mixture was cooled
4. concentrationconcentrated
5. custompartitioned between DCM and water
6. washThe organic layer was washed with water, brine solution
7. dry with materialdried over Na2SO4
8. concentrationconcentrated
9. customThe solid formed
10. customwas collected
11. washwashed with hexane and ether