反应详情

A solution of tert-butyl ((3R,4S)-4-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)tetrahydrofuran-3-yl)carbamate (1.097 g, 2.049 mmol) in DCM (15 mL, 0.137 M) and TFA (11.7 g, 102 mmol) was stirred about 40 minutes at room temperature. The excess solvents were removed under reduced pressure. The yellow oil was dissolved into DCM (˜60 mL) and washed with aqueous 1N NaOH (˜30 mL). The aqueous layer was then diluted with brine (˜15 mL) and extracted with fresh DCM (3×30 mL). The combined organic layers were dried over sodium sulfate, filtered, concentrated down, and dried to yield (3S,4R)—N3-(6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)tetrahydrofuran-3,4-diamine as a very light yellow foam (0.879 g, 99%).

1. customThe excess solvents were removed under reduced pressure
2. dissolutionThe yellow oil was dissolved into DCM (˜60 mL)
3. washwashed with aqueous 1N NaOH (˜30 mL)
4. additionThe aqueous layer was then diluted with brine (˜15 mL)
5. extractionextracted with fresh DCM (3×30 mL)
6. dry with materialThe combined organic layers were dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated down
9. customdried