CN106478638A - A kind of preparation method of 2 hydroxyl 7 Methylimidazole. simultaneously [1,2 a] pyrimidine - Google Patents
A kind of preparation method of 2 hydroxyl 7 Methylimidazole. simultaneously [1,2 a] pyrimidine Download PDFInfo
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- CN106478638A CN106478638A CN201610796786.1A CN201610796786A CN106478638A CN 106478638 A CN106478638 A CN 106478638A CN 201610796786 A CN201610796786 A CN 201610796786A CN 106478638 A CN106478638 A CN 106478638A
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- China
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- preparation
- reaction
- reaction system
- methylimidazole
- pyrimidine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/02—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains two hetero rings
- C07D487/04—Ortho-condensed systems
Abstract
The invention discloses a kind of preparation method of 2 hydroxyl 7 Methylimidazole. simultaneously [1,2 a] pyrimidine, described preparation method comprises the steps:Step a, in reaction vessel add dehydrated alcohol, 2 amino 4 methylpyrimidine, stir, in reaction system, be then slowly added to bromoacetate, reaction system heating reflux reaction;Step b, reaction system are directly evaporated to dry, obtain product.By the way, preparation method of the present invention is simple to operate, only single step reaction can achieve, and easily realizes industrialization, and meets green chemistry process requirement.
Description
Technical field
The present invention relates to medicine intermediate synthesis field and in particular to a kind of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] is phonetic
The preparation method of pyridine.
Background technology
As important medicine intermediate, the preparation of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] pyrimidine is extensively closed always
Note, the more synthesis with regard to this product.But most of synthetic route reactions are complicated, impurity that is introducing is more, and reaction condition is bad
Control, and yield is low.
Content of the invention
Present invention aim at disclosing a kind of preparation method of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] pyrimidine, this preparation
Method is simple to operate, only single step reaction can achieve, and easily realizes industrialization, and meets green chemistry process requirement.
Specific disclosure of the present invention is as follows:A kind of preparation method of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] pyrimidine,
Described preparation method comprises the steps:
Step a, in reaction vessel add dehydrated alcohol, 2- amino -4- methylpyrimidine, stir, then to reaction
It is slowly added to bromoacetate, reaction system heating reflux reaction in system;
Step b, reaction system are directly evaporated to dry, obtain product.
Preferably, in described step a, 2- amino -4- methylpyrimidine is 1 with the amount ratio of bromoacetate:(1-3).
Preferably, described 2- amino -4- methylpyrimidine and the amount ratio of bromoacetate are 1:(1-2).
Preferably, described amount ratio is mol ratio.
Preferably, reaction system heating reflux reaction 4 hours in described step a.
The invention has the beneficial effects as follows:The preparation method of 2- hydroxyl -7- Methylimidazole. of the present invention simultaneously [1,2-a] pyrimidine, behaviour
Make simple, easily-controlled reaction conditions, product high income, easily realize industrialization, and meet green chemistry process requirement.
Specific embodiment
Below presently preferred embodiments of the present invention is described in detail so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that apparent clearly defining thus making to protection scope of the present invention.
Embodiment 1:A kind of preparation method of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] pyrimidine, described preparation method includes
Following steps:
Step a, in reaction vessel add dehydrated alcohol, 2- amino -4- methylpyrimidine, stir, then to reaction
It is slowly added to bromoacetate, reaction system heating reflux reaction in system;
Step b, reaction system are directly evaporated to dry, obtain product.
Embodiment 2:A kind of preparation method of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] pyrimidine, described preparation method includes
Following steps:
Step a, in reaction vessel add dehydrated alcohol, 2- amino -4- methylpyrimidine, stir, then to reaction
It is slowly added to bromoacetate, reaction system heating reflux reaction 4 hours in system;2- amino -4- methylpyrimidine and bromoacetic acid
The mol ratio of ethyl ester is 1:(1-3).
Step b, reaction system are directly evaporated to dry, obtain product.
Embodiment 3:A kind of preparation method of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] pyrimidine, described preparation method includes
Following steps:30mL dehydrated alcohol, 1g 2- amino -4- methyl is added toward in the round-bottomed flask of the 100mL being connected to reflux condensing tube
Pyrimidine, stirring, it is then slowly added into 1.83g bromoacetate, then whole system is heated to back flow reaction 4 hours.Entirely anti-
Answer system to be directly evaporated to and dry can get purity good product 1.36g.This embodiment yield 100%.Wherein, 2- ammonia
Base -4- methylpyrimidine:Bromoacetate=1:1.2 (mol ratios).
The foregoing is only embodiments of the invention, not thereby limit the present invention the scope of the claims, every using this
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of 2- hydroxyl -7- Methylimidazole. simultaneously [1,2-a] pyrimidine is it is characterised in that described preparation method bag
Include following steps:
Step a, in reaction vessel add dehydrated alcohol, 2- amino -4- methylpyrimidine, stir, then to reaction system
In be slowly added to bromoacetate, reaction system heating reflux reaction;
Step b, reaction system are directly evaporated to dry, obtain product.
2. preparation method according to claim 1 is it is characterised in that in described step a, 2- amino -4- methylpyrimidine with
The amount ratio of bromoacetate is 1:(1-3).
3. preparation method according to claim 2 is it is characterised in that described 2- amino -4- methylpyrimidine and bromoacetic acid second
The amount ratio of ester is 1:(1-2).
4. preparation method according to claim 2 is it is characterised in that described amount ratio is mol ratio.
5. preparation method according to claim 1 is it is characterised in that reaction system heating reflux reaction 4 in described step a
Hour.
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CN201610796786.1A CN106478638A (en) | 2016-08-31 | 2016-08-31 | A kind of preparation method of 2 hydroxyl 7 Methylimidazole. simultaneously [1,2 a] pyrimidine |
Applications Claiming Priority (1)
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CN201610796786.1A CN106478638A (en) | 2016-08-31 | 2016-08-31 | A kind of preparation method of 2 hydroxyl 7 Methylimidazole. simultaneously [1,2 a] pyrimidine |
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CN106478638A true CN106478638A (en) | 2017-03-08 |
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CN201610796786.1A Pending CN106478638A (en) | 2016-08-31 | 2016-08-31 | A kind of preparation method of 2 hydroxyl 7 Methylimidazole. simultaneously [1,2 a] pyrimidine |
Country Status (1)
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CN (1) | CN106478638A (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1531540A (en) * | 2001-01-30 | 2004-09-22 | ������ҩ��ҵ��ʽ���� | Heterocyclic compounds and cerebral function improvers containing same as active |
WO2008045688A1 (en) * | 2006-10-06 | 2008-04-17 | Boehringer Ingelheim International Gmbh | Chymase inhibitors |
-
2016
- 2016-08-31 CN CN201610796786.1A patent/CN106478638A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1531540A (en) * | 2001-01-30 | 2004-09-22 | ������ҩ��ҵ��ʽ���� | Heterocyclic compounds and cerebral function improvers containing same as active |
WO2008045688A1 (en) * | 2006-10-06 | 2008-04-17 | Boehringer Ingelheim International Gmbh | Chymase inhibitors |
Non-Patent Citations (1)
Title |
---|
ESPERANCE MOINE, ET AL.: "Development of new highly potent imidazo[1,2-b]pyridazines targeting Toxoplasma gondii calcium-dependent protein kinase 1", 《EUROPEAN JOURNAL OF MEDICINAL CHEMISTRY》 * |
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Application publication date: 20170308 |