反应详情

A slurry of methyl 5-(4-chlorobenzyloxy)-2-pyridylcarbamate (0.75 g, 2.6 mmol) in 10% sodium hydroxide (20 ml) and methanol (40 ml) is heated to 90° under nitrogen gas. After 1 hour, 10 ml of 10% sodium hydroxide and 10 ml of methanol are added. Heating is continued, and after 2 hours, 10 ml of methanol is added. The reaction is heated under reflux overnight. The reaction is then rotoevaporated, and chloroform and water are added. The residue is extracted with chloroform (4×). The combined chloroform extracts are washed with water until neutral and with brine, dried over calcium sulfate, filtered and rotoevaporated to yield 2-amino-5-(4-chlorobenzyloxy)pyridine.

1. temperatureHeating
2. waitafter 2 hours
3. temperatureThe reaction is heated
4. temperatureunder reflux overnight
5. extractionThe residue is extracted with chloroform (4×)
6. washThe combined chloroform extracts are washed with water until neutral and with brine
7. dry with materialdried over calcium sulfate
8. filtrationfiltered