Synthetic method of methyl 4-methoxyacetoacetate
A technology of methyl methoxy acetoacetate and a synthesis method, applied in the field of synthesis of methyl 4-methoxy acetoacetate, can solve problems such as expensive and unaffordable molecular distillation equipment, achieve safe use and reduce usage , saving and using simple effects
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[0022] Example 1
[0023] Add 250 mL of tetrahydrofuran to the 2L reaction flask in advance, start stirring under the protection of argon, at this time the internal temperature is 25 °C, and 30 g (0.74 mol) of sodium hydride (containing 40wt%) is added in batches under the condition of the internal temperature of 15-25 °C Mineral oil) and 50g (0.74mol) potassium methoxide, continue to add 450mL of tetrahydrofuran after the addition; slowly dropwise add a mixed solution of 30g methanol and 100g (0.67mol) methyl 4-chloroacetoacetate at an internal temperature of 20°C, Adjust the stirring speed at about 310 rpm, and finish adding in about 4 hours; the internal temperature rises to 20-25 °C and stir for 5 hours. TLC detects that the reaction of the raw materials is complete, and the system begins to cool down. It can be seen that the color of the solution is light yellow and a large amount of solids are suspended. Add 200 mL of tetrahydrofuran at a temperature of 11 °C, and when t...
Example Embodiment
[0024] Example 2
[0025] Add 250 mL of tetrahydrofuran to the 2L reaction flask in advance, start stirring under the protection of argon, at this time the internal temperature is 25 °C, and 30 g (0.74 mol) of sodium hydride (containing 40wt% of minerals) are added in batches under the condition of the internal temperature of 15-25 °C oil) and 50g (0.74mol) potassium methoxide, after adding, continue to add 450mL of tetrahydrofuran; under the condition of internal temperature of 20℃, slowly add the mixed solution of 30g methanol and 100g (0.67mol) methyl 4-chloroacetoacetate dropwise, adjust The stirring rate is about 310 rpm, and the addition is completed in about 4 hours; the internal temperature rises to 20-25 °C and stirs for 5 hours, TLC detects that the reaction of the raw materials is complete; Add 200 mL of tetrahydrofuran under the condition of 11 °C, and when the internal temperature drops to -2 °C, slowly add 100 mL of hydrochloric acid solution with a molar concent...
Example Embodiment
[0026] Example 3
[0027]Add 250 mL of tetrahydrofuran to the 2L reaction flask in advance, start stirring under the protection of argon, at this time the internal temperature is 25 °C, and 30 g (0.74 mol) of sodium hydride (containing 40wt% of minerals) are added in batches under the condition of the internal temperature of 15-25 °C oil) and 50g (0.74mol) potassium methoxide, after the addition, continue to add 450mL of tetrahydrofuran, and slowly add a mixed solution of 30g methanol and 100g (0.67mol) methyl 4-chloroacetoacetate dropwise at an internal temperature of 20°C to adjust The stirring rate was about 310 rpm, and the addition was completed in about 4 hours; the internal temperature was raised to 20-25 °C and stirred for 5 hours, and TLC detected that the reaction of the raw materials was complete; Add 200 mL of tetrahydrofuran under the condition of 11 °C, and when the internal temperature drops to -2 °C, slowly add 100 mL of hydrochloric acid solution with a molar ...
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