反应详情

Cocaine (Merck) (3.91 g) was dissolved in 100 ml IN HCl and heated to reflux for 19 hours. After cooling to room temperature, the benzoic acid was filtered and washed with water. The water was washed with chloroform several times and the water was removed in vacuo. The residue was dissolved in 200 ml anhydrous methanol and the solution was saturated with HCl gas. The reaction mixture was refluxed for 17 hours. After cooling to room temperature, the solvent was removed in vacuo. The residue was dissolved in water and basified with potassium carbonate to pH 9. The basic water was extracted with methylene chloride several times. After drying the organic layer over sodium sulfate, the solvent was removed in vacuo to yield ecgonine methyl ester as an oil.

1. temperatureheated
2. temperatureto reflux for 19 hours
3. filtrationthe benzoic acid was filtered
4. washwashed with water
5. washThe water was washed with chloroform several times
6. customthe water was removed in vacuo
7. dissolutionThe residue was dissolved in 200 ml anhydrous methanol
8. temperatureThe reaction mixture was refluxed for 17 hours
9. temperatureAfter cooling to room temperature
10. customthe solvent was removed in vacuo
11. dissolutionThe residue was dissolved in water
12. extractionThe basic water was extracted with methylene chloride several times
13. dry with materialAfter drying the organic layer over sodium sulfate
14. customthe solvent was removed in vacuo