A kind of method for preparing saxagliptin intermediate
A technology for intermediates and acetonitrile, applied in the field of preparing saxagliptin intermediates, can solve problems such as unfavorable large-scale production and environmental protection, low yield, complicated post-reaction treatment, etc., achieve stable yield and improve product yield and purity, high yield effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0027]
[0028] 2.5kg of acetonitrile, 1.77kg of ethyl acetate, and 2.03kg of N,N-diisopropylethylamine were successively added to the reaction kettle, and the mixture was stirred for use. Then add 2.33kg of raw material A, 1.67kg of saxagliptin intermediate 1, 1.11kg of hydroxybenzotriazole, 1.51 kg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride kg, 2.83 kg of acetonitrile, stirred for 2-3 hours.
[0029] After distilling off most of the acetonitrile under reduced pressure, 20.90 kg of ethyl acetate was added to the reaction solution and stirred. After adjusting the pH to neutrality, 11.80 kg of sodium chloride solution was added, stirred at room temperature, and the aqueous layer was removed after standing. 12.76 kg of 20% potassium bicarbonate solution was added to the organic phase, stirred, and the aqueous layer was removed after standing. 12.76 kg of 20% potassium bicarbonate solution was added to the organic phase and stirred, and the aqueous layer ...
Embodiment 2
[0032]
[0033] 10kg of acetonitrile, 7.1kg of ethyl acetate, 8.1kg of N,N-diisopropylethylamine were successively added to the reaction kettle, and the mixture was stirred for use. Then add 9.32kg of raw material A, 6.68kg of saxagliptin intermediate 1, 4.4kg of hydroxybenzotriazole, 6.0kg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride kg, 11.3 kg of acetonitrile, and stirred for 3 hours.
[0034] After most of the acetonitrile was distilled off under reduced pressure, 83.6 kg of ethyl acetate was added to the reaction solution and stirred. After the pH was adjusted to neutral, 47.2 kg of sodium chloride solution was added, stirred at room temperature, and the aqueous layer was removed after standing. 51.0 kg of 20% potassium bicarbonate solution was added to the organic phase, stirred, and the aqueous layer was removed after standing.
[0035] The organic phase was desolvated to 16-25L under reduced pressure, and 23.2 kg of ethyl acetate was added, and t...
Embodiment 3
[0037]
[0038] 25.0 g of acetonitrile, 17.7 g of ethyl acetate, and 20.3 g of N,N-diisopropylethylamine were successively added to the reactor, and the mixture was stirred for use. Next, 3.3 g of raw material A, 16.8 g of saxagliptin intermediate 1, 11.12 g of hydroxybenzotriazole, and 15.1 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added in sequence. g, 28.3 g of acetonitrile, and stirred for 2 hours.
[0039] To the reaction liquid was added 209.0 g of ethyl acetate and stirred. After the pH was adjusted to neutral, 118.0 g of sodium chloride solution was added, stirred at room temperature, and the aqueous layer was removed after standing. 127.6 g of 20% potassium bicarbonate solution was added to the organic phase and stirred, and the aqueous layer was removed after standing. 127.6 g of 20% potassium bicarbonate solution was added to the organic phase and stirred, and the aqueous layer was removed after standing.
[0040] The organic phase ...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More