A kind of synthetic method of palbociclib intermediate
A synthetic method and intermediate technology, applied in the field of palbociclib intermediates, can solve the problems of complex steps, unsuitability for industrial production, and low product yield, and achieve simple operation, high product yield, and easy-to-obtain raw materials Effect
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Embodiment 1
[0028] 1) Preparation of compound II
[0029] Dissolve 341.7 g of compound I into 1800 g of tetrahydrofuran in two steps, that is, the first time is 150 g of compound I+800 g of tetrahydrofuran, and the second is 191.7 g of compound I+1000 g of tetrahydrofuran.
[0030] 1800g of tetrahydrofuran was added to the reaction flask, 45g of magnesium scraps were put in, 1 iodine was added, 150g of the tetrahydrofuran solution of compound I was added dropwise to the Grignard flask under nitrogen protection, the temperature was raised to 30°C, and the remaining compounds were added after the reaction was initiated. The tetrahydrofuran solution of I was added dropwise to the Grignard reaction flask at a controlled temperature of 25-32°C, and continued stirring at this temperature for 2 hours after dropping. Control the temperature to -10-0°C, add 165g of trimethyl borate dropwise to the Grignard reaction flask, complete the dropwise addition and react for 30 minutes, control the materia...
Embodiment 2
[0035] 1) Preparation of compound II
[0036] 341.7 g of compound I was dissolved in 1500 g of tetrahydrofuran in two times, that is, the first time was 150 g of compound I+600 g of tetrahydrofuran, and the second time was 191.7 g of compound I+900 g of tetrahydrofuran.
[0037] 1500g of tetrahydrofuran was added to the reaction flask, 42g of magnesium scraps were put in, 1 iodine was added, 150g of the tetrahydrofuran solution of compound I was added dropwise to the Grignard flask under nitrogen protection, the temperature was raised to 30°C, and the remaining compounds were added after the reaction was initiated. The tetrahydrofuran solution of I was added dropwise to the Grignard reaction flask at a temperature of 25-32°C, and continued stirring at this temperature for 2.5 hours after dropping. Control the temperature to -10-0°C, add 163g of trimethyl borate into the Grignard reaction flask, dropwise and react for 35 minutes, control the material to 0-10°C, add it to 12kg o...
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