反应详情

温度

0 °C

A suspension of 750 mg (15.77 mmol) of sodium hydride in 50 mL of DMF is cooled to 0° C. under argon. A solution of 2 g (7.89 mmol) of (8S)-2-chloro-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one in 50 mL of DMF is added dropwise. The mixture is stirred for 10 minutes at room temperature. After cooling the reaction medium to 0° C., 2.92 g (9.86 mmol) of 3-(bromoacetyl)pyridine hydrobromide are added portionwise. The reaction mixture is allowed to warm to room temperature and is stirred overnight. The reaction medium is evaporated to dryness and the residue is taken up in water and extracted with EtOAc. The organic phase is dried over magnesium sulfate and evaporated to dryness. The crude product obtained is purified by chromatography on silica gel (eluent: 100% EtOAc). After evaporating the fractions under reduced pressure, 1.90 g of (8S)-2-chloro-9-(2-oxo-2-pyrid-3-ylethyl)-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one are obtained, the characteristics of which are as follows:

1. temperatureAfter cooling the reaction medium to 0° C.
2. temperatureto warm to room temperature
3. stirringis stirred overnight
4. customThe reaction medium is evaporated to dryness
5. extractionextracted with EtOAc
6. dry with materialThe organic phase is dried over magnesium sulfate
7. customevaporated to dryness