反应详情

A solution of 6-nitro-2,2-dimethyl-2H-benzopyran (prepared as described in Evans et al., J. Med. Chem.) (4.65 g, 22.66 mmoles) and SnCl2. 2H2O (25.57 g, 0.11 mole) in ethanol (46.5 ml) was heated at reflux for 45 minutes. The reaction mixture was poured onto ice/H2O (180 g), made basic (pH 10-11) with 50% sodium hydroxide solution, and extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution, dried over sodium sulfate, and evaporated in vacuo to obtain 3.88 g of the title A compound as a brown oil.

1. temperatureat reflux for 45 minutes
2. additionThe reaction mixture was poured onto ice/H2O (180 g)
3. extractionextracted with ethyl acetate
4. washThe organic phase was washed with saturated sodium chloride solution
5. dry with materialdried over sodium sulfate
6. customevaporated in vacuo