反应详情

温度

-78 °C

Ph3P (0.213 g, 0.812 mmol) was taken up in THF (6 ml) and cooled to −78° C. under N2. DIAD (0.126 ml, 0.650 mmol) was added followed by addition of phthalimide (0.105 g, 0.711 mmol) and stirred at −78° C. for 1 hour, followed by addition of (1S,3R,4R)-methyl 3-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)-4-hydroxycyclopentanecarboxylate (0.100 g, 0.203 mmol) in 4 ml of THF at −78° C. The reaction was stirred overnight while warming to room temperature, after which the solvent was removed under reduced pressure. The residue was purified via flash chromatography (0-100% Hex/EtOAc; 12 g column) to afford methyl (3R,4S)-3-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)-4-(1,3-dioxoisoindolin-2-yl)cyclopentane-1-carboxylate (0.126 g, 0.203 mmol). MS (ES+) C31H26Cl2N4O6 requires: 621, found: 622 [M+H]+.

1. stirringThe reaction was stirred overnight
2. temperaturewhile warming to room temperature
3. customafter which the solvent was removed under reduced pressure
4. customThe residue was purified via flash chromatography (0-100% Hex/EtOAc; 12 g column)