Preparation method of apoate key intermediate C10 aldehyde ester
The technology of an intermediate and apoester is applied in the synthesis field of the key intermediate C10 aldehyde ester, can solve the problems of high process cost, difficult industrialization, low yield and the like, and achieves low process cost, few by-products, and excellent yield. Effect
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Embodiment 1
[0043] Synthesis of C6 Dialdehydes:
[0044] 10g of acetoacetaldehyde and 80g of n-butanol were added to the reactor, nitrogen was replaced three times, the temperature of the reaction solution was lowered to -5°C, 10g of bis(trimethylsilyl) potassium amide was added, and then the dropwise addition of glyoxal was started. Diethyl ether solution (40% concentration) 30g, the dropwise addition time is 2h, after the dropwise addition is completed, the reaction is kept at 20 ° C for 30min, and the acetoacetaldehyde conversion rate in the reaction solution is sampled and analyzed > 99%, this step reaction ends; the reaction solution The continuous vacuum distillation method is used for separation, and the control distillation conditions are: the pressure is 15kPa, the temperature of the tower is 65°C, the number of trays is 15, the reflux ratio is 9, and the top of the tower can obtain C6 bicarbonate with a purity of 93.6%. Aldehyde intermediate, the yield of this step is 85%.
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Embodiment 2
[0048]Synthesis of C6 Dialdehydes:
[0049] 10g of acetoacetaldehyde and 50g of acetonitrile were added to the reactor, nitrogen was replaced three times, the temperature of the reaction solution was lowered to 0°C, 12g of bis(trimethylsilyl) potassium amide was added, and then the ether solution of glyoxal was added dropwise ( 40% concentration) 52g, the dropwise addition time is 3h, after the dropwise addition is completed, the reaction is kept at 15°C for 30min, and the conversion rate of acetoacetaldehyde in the reaction solution is sampled and analyzed > 99%, and this step of the reaction is completed; The pressure distillation method is used for separation, and the control distillation conditions are as follows: the pressure is 15kPa, the temperature of the tower still is 80°C, the number of trays is 12, the reflux ratio is 6, and the C6 dialdehyde intermediate with a purity of 91.8% can be obtained at the top of the tower. , the yield of this step is 86.8%.
[0050] Sy...
Embodiment 3
[0053] Synthesis of C6 Dialdehydes:
[0054] 10g of acetoacetaldehyde and 100g of methanol were added to the reactor, nitrogen was replaced three times, the temperature of the reaction solution was lowered to 0°C, 11g of bis(trimethylsilyl) sodium amide was added, and then the ether solution of glyoxal was added dropwise ( 40% concentration) 50g, the dropwise addition time is 4h, after the dropwise addition is completed, the reaction is kept at 20°C for 30min, and the conversion rate of acetoacetaldehyde in the reaction solution is sampled and analyzed >99%, and this step of the reaction is completed; The pressure rectification method is used for separation, and the control rectification conditions are: the pressure is 12kPa, the temperature of the tower reactor is 50°C, the number of trays is 20, the reflux ratio is 10, and the C6 dialdehyde intermediate with a purity of 92.0% can be obtained at the top of the tower. , the yield of this step was 87.5%.
[0055] Synthesis of ...
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