反应详情

温度

100 °C

Amphetamine free base (100 mg, 0.71 mmol) was dissolved in ethyl formate (10 mL). The solution was heated under pressure in an ACE pressure reactor for 2 hours at 100° C. The reaction mixture was cooled to ambient temperature, and the solvent was evaporated under reduced pressure. The resulting carbamate derivative was dissolved in dried diethyl ether (5 mL). The solution was added dropwise to a suspension of lithium aluminium hydride (40.4 mg, 1.07 mmol) in dry diethyl ether (10 mL). The reaction mixture was refluxed for 5 hours. Thereafter, water was carefully added after the reaction mixture had been cooled down to 0° C. on an ice bath. The lithium salt was filtered over Celite™ diatomaceous earth in a Buchner funnel. The granules obtained were washed thoroughly with excess diethyl ether. The combined ether phases were washed with 5% sodium hydroxide and brine before being dried over magnesium sulfate. The solvent was evaporated to yield 96 mg methamphetamine free base.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. customthe solvent was evaporated under reduced pressure
3. dissolutionThe resulting carbamate derivative was dissolved in dried diethyl ether (5 mL)
4. temperatureThe reaction mixture was refluxed for 5 hours
5. temperaturehad been cooled down to 0° C. on an ice bath
6. filtrationThe lithium salt was filtered over Celite™ diatomaceous earth in a Buchner funnel
7. customThe granules obtained
8. washwere washed thoroughly with excess diethyl ether
9. washThe combined ether phases were washed with 5% sodium hydroxide and brine
10. dry with materialbefore being dried over magnesium sulfate
11. customThe solvent was evaporated