Synthetic method for 2-pyridylcarbinol
A technology of pyridinemethanol and synthetic method, which is applied in the direction of organic chemistry, can solve the problems of low product purity, complex post-processing, and many reaction by-products, and achieve the effects of accelerating the reaction rate, shortening the reaction time, high yield and purity
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Embodiment 1
[0026] The synthetic method of 2-pyridinemethanol is characterized in that, comprises the following steps of synthesis:
[0027] 1) Synthesis of 2-methyl-3,5-dinitropyridine
[0028] Take 23.25g of 2-methylpyridine as the synthetic raw material, add 24.8ml of 98% concentrated sulfuric acid to it, stir and raise the temperature to 70°C, then add 75.6ml of mixed acid to it dropwise, after the dropwise addition, raise the temperature to 90-92°C and keep it warm for 2.2h , then cooled in an ice-water bath, and 250mL of ice water was added thereto, 23.2g of 30% sodium hydroxide solution was added dropwise for neutralization, stirred for 1.5h, and then extracted with ethyl acetate, the solvent was recovered by distillation under reduced pressure, and an organic reagent was used to Recrystallize, filter and dry to obtain 43.21 g of 2-methyl-3,5-dinitropyridine with a yield of 94.4%;
[0029] 2) Synthesis of 2-methyl-3,5-dinitropyridine-N-oxide
[0030] Take 36.62g of 2-methyl-3,5-d...
Embodiment 2
[0036] The synthetic method of 2-pyridinemethanol is characterized in that, comprises the following steps of synthesis:
[0037] 1) Synthesis of 2-methyl-3,5-dinitropyridine
[0038] Take 18.6g of 2-methylpyridine as the synthetic raw material, add 19.2ml of 98% concentrated sulfuric acid to it, stir and raise the temperature to 70°C, then add 58.7ml of mixed acid dropwise therein, after the dropwise addition, raise the temperature to 90-92°C and keep it warm for 2.5h , then cooled in an ice-water bath, and 250mL of ice water was added thereto, 18.2g of 30% sodium hydroxide solution was added dropwise for neutralization, stirred for 1h, and then extracted with ethyl acetate, the solvent was recovered by distillation under reduced pressure, and carried out with organic reagents Recrystallized, filtered and dried to obtain 35.19 g of 2-methyl-3,5-dinitropyridine with a yield of 96.1%;
[0039] 2) Synthesis of 2-methyl-3,5-dinitropyridine-N-oxide
[0040] Take 29.3g of 2-methyl...
Embodiment 3
[0046] The synthetic method of 2-pyridinemethanol is characterized in that, comprises the following steps of synthesis:
[0047] 1) Synthesis of 2-methyl-3,5-dinitropyridine
[0048] Take 32.74g of 2-methylpyridine as the synthetic raw material, add 31.5ml of 98% concentrated sulfuric acid into it, stir and heat up to 70°C, then add 100ml of mixed acid dropwise therein, after the dropwise addition, raise the temperature to 90-92°C and keep it warm for 1.8h. Then it was cooled in an ice-water bath, and 250mL of ice water was added thereto, and 32.6g of 30% sodium hydroxide solution was added dropwise for neutralization, stirred for 1h, then extracted with ethyl acetate, the solvent was recovered by distillation under reduced pressure, and an organic reagent was used to regenerate Crystallized, filtered and dried to obtain 52.35 g of 2-methyl-3,5-dinitropyridine with a yield of 95.3%;
[0049] 2) Synthesis of 2-methyl-3,5-dinitropyridine-N-oxide
[0050] Take 45.78g of 2-methy...
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