反应详情

温度

120 °C

A suspension of 2,4-difluorobenzonitrile (1 g, 7.17 mmol), formamidine acetate (2.98 g, 28.68 mmol), and NaH (60% suspension in mineral oil, 2.29 g, 57.36 mmol) in dimethylacetamide (50 mL) is stirred at 120° C. for overnight. The reaction mixture is poured onto a saturated solution of NaHCO3 (100 mL), and the aqueous phase is extracted with EtOAc (3×). The combined organic layers is washed with brine, dried over MgSO4, and evaporated to dryness. Purification of the crude material by column chromatography (10% MeOH in CH2Cl2) affords 7-Fluoro-quinazolin-4-ylamine (0.2874 g, 25%). LC/MS m/z=164 [M+H]+.

1. extractionthe aqueous phase is extracted with EtOAc (3×)
2. washThe combined organic layers is washed with brine
3. dry with materialdried over MgSO4
4. customevaporated to dryness
5. customPurification of the crude material by column chromatography (10% MeOH in CH2Cl2)