Preparation method of serinol by normal-pressure catalytic reduction
A technology of serinol and atmospheric pressure, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc. It can solve the problems of inconvenient post-processing, danger, and influence on product quality, and achieve cheap catalysts. , cost reduction effect
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Embodiment １
[0030] Add 1200 g of methanol into a 2000 ml reaction flask, add 200 g of the main raw material 5-nitro-2,2-dimethyl-1,3-dioxane (I), and then add 4 g of Raney nickel, Start stirring to keep the temperature in the reaction bottle between 60 and 65°C, slowly add 135g of hydrazine hydrate with a mass concentration of 80%, and keep it warm for 3 hours. After the catalytic reduction is completed, filter out Raney nickel, which can Repeatedly used to the next batch, the methanol was evaporated to dryness under reduced pressure to obtain the intermediate product (II), and then 400 g of dilute hydrochloric acid with a mass concentration of 18% was added to hydrolyze to obtain the crude product of serinol, and then recrystallized to obtain about 95 g of silk Amino alcohol, the GC purity is about 99.8% by sampling.
Embodiment 2
[0032] Add 1100 g of ethanol to a 2000 ml reaction bottle, add 200 g of the main raw material 5-nitro-2,2-dimethyl-1,3-dioxane (I), and then add 6 g of Raney nickel, Start stirring to keep the temperature in the reaction bottle between 70~75°C, slowly add 150 g of hydrazine hydrate with a mass concentration of 80% dropwise, keep the temperature for 5 hours, and filter out Raney nickel and Raney nickel after the catalytic reduction is completed. It can be reused in the next batch. The intermediate product (II) is obtained by evaporating ethanol under reduced pressure, and then adding 400 g of dilute hydrochloric acid with a mass concentration of 20% for hydrolysis to obtain the crude product of serinol, and then recrystallizing to obtain about 92 g Serinol, the GC purity is about 99.7% by sampling.
Embodiment 3
[0034] Add 1000 g of ethyl acetate to a 2000 ml reaction bottle, add 200 g of the main raw material (I), then add 6 g of Raney nickel, start stirring, keep the temperature in the reaction bottle between 70~75 °C, slowly drop Add 180 g of hydrazine hydrate with a mass concentration of 80%, keep the temperature for 8 hours, and filter out Raney nickel after the catalytic reduction is completed. The Raney nickel can be reused in the next batch, and the ethyl acetate is evaporated under reduced pressure to obtain the intermediate product ( Ⅱ), and then add 500 g of dilute hydrochloric acid with a mass concentration of 15% for hydrolysis to obtain a crude serinol product, and then recrystallize to obtain about 81 g of serinol, and the GC purity of the sample is about 99.5%.
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