反应详情

温度

80 °C

A 1.00 g portion of methyl 5-amino-2,4-dimethoxybenzoate was dissolved in 5 ml of water, 0.50 ml of concentrated sulfuric acid was added and then 356 mg of sodium nitrite dissolved in 2 ml of water was added dropwise under ice-cooling, followed by a short period of stirring. Separately, 1.00 g of cuprous cyanide was dissolved in 4 ml of water and, with ice-cooling, 2.00 g of sodium cyanide dissolved in 4 ml of water was added dropwise thereto, followed by 1 hour of stirring. This was mixed with the previously prepared solution and heated at 80° C. to effect the reaction, the resulting reaction solution was mixed with water, extracted with chloroform and dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure and then the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=6:1 to chloroform:methanol=50:1) to give 0.65 g of methyl 5-cyano-2,4-dimethoxybenzoate.

1. additionwas added dropwise under ice-
2. temperaturecooling
3. waitfollowed by a short period
4. temperaturecooling
5. additionwas added dropwise
6. stirringof stirring
7. additionThis was mixed with the previously prepared solution
8. customthe reaction
9. customthe resulting reaction solution
10. extractionextracted with chloroform
11. dry with materialdried over anhydrous sodium sulfate
12. customThe solvent was evaporated under a reduced pressure
13. customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=6:1 to chloroform:methanol=50:1)