反应详情

A solution of 3-dimethylaminomethylene-6-methyl-pyran-2,4-dione (preparation 1a, 10.00 g, 38.6 mmol based on 70% purity), isopropylamine (5.00 mL, 58.4 mmol) and sodium tert-butoxide (5.50 g, 57.2 mmol) in ethanol (20 mL) is heated for 18 h at 90° C. The reaction mixture is evaporated under reduced pressure, treated with water and extracted with dichloromethane. The aqueous layer is acidified with 4 N aqueous HCl and extracted with dichloromethane. The combined organic layer is washed with water, dried over Na2SO4 and evaporated under reduced pressure. Yield: 7.16 g; ESI mass spectrum: [M+H]+=196; r.t. HPLC: 0.71 min (Z002_006).

1. customThe reaction mixture is evaporated under reduced pressure
2. additiontreated with water
3. extractionextracted with dichloromethane
4. extractionextracted with dichloromethane
5. washThe combined organic layer is washed with water
6. dry with materialdried over Na2SO4
7. customevaporated under reduced pressure
8. customr.t
9. custom0.71 min (Z002_006)