3430-34-0Relevant articles and documents
Synthesis method of 2, 6-dimethyl-3, 5-dibromopyridine
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Paragraph 0020; 0023; 0024; 0026, (2019/05/28)
The invention relates to the field of organic chemistry, in particular to a synthesis method of 2, 6-dimethyl-3, 5-dibromopyridine. The method includes following steps: (1), adding 2, 6-dimethyl-3-aminopyridine and acetic anhydride into a four-neck flask, rising temperature to backflow, and allowing thin-layer chromatography tracking reaction; (2), when temperature of reaction liquid in the step (1) is lowered to below 23 DEG C, dropwise adding liquid bromine, allowing reaction at 40-55 DEG C for 2-3h after dropwise adding is completed, adding water until all solid is dissolved, dropwise adding a sodium hydroxide solution, continuing reaction for 20-40min when a lot of precipitate is generated, suction-filtering, drying, and recrystallizing to obtain 2, 6-dimethyl-3-amino-5 bromopyridine;(3), adding 2, 6-dimethyl-3-amino-5 bromopyridine into a hydrogen bromide solution, dropwise adding a saturated sodium nitrite solution at the presence of cuprous bromide in a catalysis amount, controlling temperature to -3-4 DEG C, and allowing reaction for 2-3h to obtain 2, 6-dimethyl-3, 5-dibromopyridine.The method has the advantages of being mild in reaction condition, high in yield, easy-to-get in raw material, low in cost and short in process route and having industrialization prospect.
Synthetic method of 2,6-dimethyl-3,5-dibromopyridine
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Paragraph 0018; 0020; 0021; 0023; 0024; 0026, (2017/11/30)
The invention relates to the field of organic chemistry, in particular to a synthetic method of 2,6-dimethyl-3,5-dibromopyridine. The synthetic method comprises the following steps: (1) adding 2,6-dimethyl-3-aminopyridine and acetic anhydride into a four-necked flask, raising the temperature till backflow and performing thin layer chromatography tracking reaction; (2) after the temperature of reaction liquid in the step (1) is reduced to below 23 DEG C, dropwise adding liquid bromine, reacting for 2-3 hours at a temperature of 40-55 DEG C after the completion of dropwise adding, adding water till all solids are dissolved, then dropwise adding a sodium hydroxide solution, continuously reacting for 20-40 minutes after the generation of a large number of precipitates, performing suction filtration, drying and re-crystallizing to obtain 2,6-dimethyl-3-amino-5-bromopyridine; (3) adding the 2,6-dimethyl-3-amino-5-bromopyridine into a hydrogen bromide solution, dropwise adding a saturated sodium nitrite solution under the existence of a catalytic amount of cuprous bromide, controlling the temperature between 3 DEG C below zero and 4 DEG C and reacting for 2-3 hours to obtain the 2,6-dimethyl-3,5-dibromopyridine. The synthetic method provided by the invention is mild in reaction condition, high in yield, readily-available in raw material, lower in cost and short in process route and has an industrial prospect.