反应详情

温度

-78 °C

A mixture of CuI (152 mg, 0.8 mmol) and isopropylmagnesium bromide (1.6 ml, 1.6 mmol; 1.0M in THF) in anhydrous THF (5 ml) was stirred at −78° C. for 30 minutes. To this mixture was added a solution of 2,4-dichloro-6-(4-fluoro-phenyl)-pyrido[3,2-d]pyrimidine (60 mg, 0.2 mmol) in THF (4 ml). The resulting mixture was stirred at −78° C. for another 2 hours before warming up to room temperature. The reaction was quenched by adding a solution of saturated aqueous ammonium chloride and concentrated ammonia (4:1 ratio; 5 ml). The mixture was extracted with EtOAc and the extracts dried over Na2SO4. Solvents were concentrated in vacuo and the crude residue was used in the next step without further purification. The resulting compound was characterized as follows: MS (m/z) 302.1 [M+H]+; HPLC Rt=4.72 minutes (Method A).

1. stirringThe resulting mixture was stirred at −78° C. for another 2 hours
2. temperaturebefore warming up to room temperature
3. customThe reaction was quenched
4. additionby adding a solution of saturated aqueous ammonium chloride and concentrated ammonia (4:1 ratio; 5 ml)
5. extractionThe mixture was extracted with EtOAc
6. dry with materialthe extracts dried over Na2SO4
7. concentrationSolvents were concentrated in vacuo
8. customthe crude residue was used in the next step without further purification