反应详情

Hydrogen chloride gas was bubbled through a −78° C. solution of tert-butyl 4-fluoro-2-[(methylamino)carbonyl]benzylcarbamate (615 mg, 2.18 mmol) in ethyl acetate (20 mL) until the solution was saturated. The flask was then allowed to warm to room temperature. The reaction was concentrated in vacud to a volume of about 5 mL and the flask was capped and placed in the freezer overnight. In the morning, the solids that had precipitated were collected by vacuum filtration and washed with cold ethyl acetate to give the desired product as an off-white solid.

1. concentrationThe reaction was concentrated in vacud to a volume of about 5 mL
2. customthe flask was capped
3. customplaced in the freezer overnight
4. customIn the morning, the solids that had precipitated
5. filtrationwere collected by vacuum filtration
6. washwashed with cold ethyl acetate