反应详情

温度

-50 °C

To a solution of 0.500 g (2.06 mmol) of 2-pyrimidin-4-yl-7,8,9,10-tetrahydro-6H-pyrimido[1,2-a]azepin-4-one (step 6.1 of example 6) in dry tetrahydrofuran (20 mL) under argon at −40° C. was added 2.27 mL (2.27 mmol) of lithium bis(trimethylsilyl)amide (1M in tetrahydrofuran). The solution was stirred at −50° C. for 10 min and 1.04 g (5.16 mmol) of 4-nitrophenyl chloroformate diluted in 3 ml of dry tetrahydrofuran was added. The mixture was quenched with the addition of a saturated solution of ammonium chloride and extracted with dichloromethane. The organic phase was dried over sodium sulfate and concentrated. The residue was used as such for the next step.

1. additionwas added
2. customThe mixture was quenched with the addition of a saturated solution of ammonium chloride
3. extractionextracted with dichloromethane
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated