Method for preparing 2-chloro-4-neopentylpyridine
A technology of pentylpyridine and hydroxyneopentyl, which is applied in the field of preparing 2-chloro-4-neopentylpyridine, can solve the problems of not preparing 2-chloro-4-neopentylpyridine and the like, achieves easy availability of raw materials, Conducive to industrial production and the effect of improving yield
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Embodiment 1-1
[0034] Preparation of 4-(2-Hydroxyneopentyl)pyridine
[0035] The present embodiment provides a kind of preparation method of 4-(2-hydroxy neopentyl) pyridine, and reaction equation is as follows:
[0036]
[0037] Concrete reaction steps are as follows:
[0038] Dissolve 4-pyridinecarbaldehyde (30g) in tetrahydrofuran (300ml) at room temperature, stir the system to dissolve, lower the temperature and control the temperature at -60~-50°C, add 1.7M tert-butylmagnesium chloride (329.5ml) dropwise, after the addition is complete, the natural Raise the temperature to 40-50°C and react for 3h. After the reaction was completed, the temperature was lowered to 0-10°C, and saturated ammonium chloride solution was added dropwise to quench the reaction, stirred for 1 h, left to stand for separation, the aqueous layer was extracted once with ethyl acetate, the organic layers were combined, and concentrated to dryness at 50°C to obtain 44.5g The light yellow solid product 4-(2-hydroxy...
Embodiment 1-2
[0040] Screening of Reaction Conditions for Preparation of 4-(2-Hydroxyneopentyl)pyridine
[0041] This embodiment further screens the reaction conditions of the preparation method of 4-(2-hydroxyneopentyl)pyridine provided in Example 1-1. Temperature control temperature, the general reaction steps are as follows:
[0042] Dissolve 4-pyridinecarbaldehyde (30g) in tetrahydrofuran (300ml) at room temperature, stir the system to dissolve, lower the temperature and control the temperature, add 1.7M tert-butylmagnesium chloride (329.5ml, 2eq) dropwise, after the dropwise addition is complete, heat up naturally, and react for 3h . After the reaction was completed, the temperature was lowered to 0-10°C, and saturated ammonium chloride solution was added dropwise to quench the reaction, stirred for 1 h, allowed to stand for separation, the aqueous layer was extracted once with ethyl acetate, the organic layers were combined, concentrated to dryness at 50°C, and column chromatography ...
Embodiment 2-1
[0048] Preparation of 4-Neopentylpyridine
[0049] The present embodiment provides a kind of preparation method of 4-neopentylpyridine, and reaction equation is as follows:
[0050]
[0051] Concrete reaction steps are as follows:
[0052] Under the protection of nitrogen, 4-(2-hydroxyneopentyl)pyridine (40g), triethylsilane (160g), and trifluoroacetic acid (120g) were added to the reaction flask, and the temperature was raised to reflux for 10 hours. The reaction of the raw materials was complete. Cool down to 50°C, add 8ml of water, adjust to alkaline (pH=9~10) with solid sodium carbonate, and then adjust the system with saturated sodium sulfite solution until the starch potassium iodide test paper no longer changes color, then add 30ml of n-hexane, stir for 1h, let stand Separate the layers, combine the organic phases, and dry over anhydrous sodium sulfate. The organic layer was concentrated to dryness. 34.1 g of oily liquid product 4-neopentylpyridine was obtained with...
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