HRID2371681
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 1.39 g of ethyl N-cyanopropionimidate, 2.17 g of 6-cyano-3,4-dihydro-2,2-dimethyl-trans-4-amino-2H-benzo[b]pyran-3-ol was added, and the mixture was reacted under stirring at a temperature of from 100° to 120° C. for 2 hours. The reaction mixture was cooled, then dissolved in 100 ml of ethyl acetate, washed twice with a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate Then, ethyl acetate was distilled off under reduced pressure The residual oily substance was purified by silica gel column chromatography to obtain 1.48 g of the above identified compound in the form of crystals.
WORKUP
后处理
- customthe mixture was reacted
- temperatureThe reaction mixture was cooled
- washwashed twice with a saturated sodium chloride aqueous solution
- dry with materialdried over anhydrous sodium sulfate
- distillationethyl acetate was distilled off under reduced pressure The residual oily substance
- customwas purified by silica gel column chromatography
- customto obtain 1.48 g of the