CN104649957A - 2,2,6,6-tetramethyl-4-pipradrol preparation method - Google Patents
2,2,6,6-tetramethyl-4-pipradrol preparation method Download PDFInfo
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- CN104649957A CN104649957A CN201310578374.7A CN201310578374A CN104649957A CN 104649957 A CN104649957 A CN 104649957A CN 201310578374 A CN201310578374 A CN 201310578374A CN 104649957 A CN104649957 A CN 104649957A
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- tetramethyl
- pipradrol
- autoclave
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D211/00—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings
- C07D211/04—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D211/06—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D211/36—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D211/40—Oxygen atoms
- C07D211/44—Oxygen atoms attached in position 4
- C07D211/46—Oxygen atoms attached in position 4 having a hydrogen atom as the second substituent in position 4
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Hydrogenated Pyridines (AREA)
Abstract
The invention discloses a preparation method of 2,2,6,6-tetramethyl-4-pipradrol, which comprises the following steps: 1)adding piperidone, a solvent and a catalyst in an autoclave having a cooling water pipe, a pressure gauge, a stirring device and a thermometer, introducing nitrogen for replacing air in the autoclave for three times, introducing hydrogen to 1 MPa, stirring and heating to 90 DEG C and reacting for 1.4 hours; 2)after the reaction is finished, cooling to 50 DEG C, emptying, taking the materials out, filtering the catalyst; 3)distilling the filtrate, recovering the solvent, cooling and crystallizing the solvent; and 4)washing crystal by using cyclohexane, and filtering to obtain the white pipradrol crystals. According to the preparation method, the mixed solvent is used, the obtained product has the advantages of high yield and high purity, and the used mixed solvent has the advantages of low cost, easily available raw material, no toxicity, easy recovery, cycle use, reduced production cost and green environmental protection.
Description
Technical field
The present invention relates to a kind of preparation method of light stabilizer intermediate, be specifically related to a kind of preparation method of 2,2,6,6-tetramethyl--4-piperidine alcohols.
Background technology
Hindered amine light stabilizer be a class have space steric effect with 2,2,6,6-tetramethyl piperidine is the compound of parent, also be a kind of new and effective photostabilizer, its effect is 2-4 times of conventional stabilizer, has good synergistic effect with UV light absorber and oxidation inhibitor simultaneously.Piperidine alcohols is the important intermediate of biosynthesis block amine photostabilizer.At present, the industrial preparative method mainly pressurized catalysis hydride process of domestic and international piperidine alcohols, the solvent used in reaction is mostly organic solvent, as toluene, tetrahydrofuran (THF), Tributyl phosphate ester, methyl alcohol, Virahol, isopropylcarbinol etc., these solvents not only price are higher, and some toxic solvent, there is pollution to environment.
Summary of the invention
The object of the invention is to, provide a kind of 2,2,6, the preparation method of 6-tetramethyl--4-piperidine alcohols, use mixed solvent, products obtained therefrom yield is high, purity is high, and, mixed solvent used easy recovery cheap and easy to get, nontoxic, to can be recycled, reduce production cost, environmental protection.
The preparation method of described 2,2,6,6-tetramethyl--4-piperidine alcohols, it comprises the following steps:
One, add in the autoclave with water-cooled tube, pressure warning unit, stirring, thermometer by piperidone, solvent, catalyzer, air three times in logical nitrogen replacement still, logical hydrogen, to 1MPa, stirs intensification 90 DEG C, reaction 1.4h;
Two, react complete, be cooled to 50 DEG C, emptying, take out material, leach catalyzer;
Three, gained filtrate is distilled, recycling design, remaining solution is carried out cool, crystallization;
Four, the white piperidine alcohols crystal above-mentioned crystallization hexanaphthene is washed, filtered refining.
The preparation method of 2,2,6,6-tetramethyl--4-piperidine alcohols provided by the invention, its beneficial effect is, use mixed solvent, products obtained therefrom yield is high, purity is high, and, mixed solvent used easy recovery cheap and easy to get, nontoxic, to can be recycled, reduce production cost, environmental protection.
Embodiment
Below in conjunction with an embodiment, the preparation method of 2,2,6,6-tetramethyl--4-piperidine alcohols provided by the invention is described in detail.
Embodiment
One, add in the autoclave with water-cooled tube, pressure warning unit, stirring, thermometer by piperidone, solvent, catalyzer, air three times in logical nitrogen replacement still, logical hydrogen, to 1MPa, stirs intensification 90 DEG C, reaction 1.4h;
Two, react complete, be cooled to 50 DEG C, emptying, take out material, leach catalyzer;
Three, gained filtrate is distilled, recycling design, remaining solution is carried out cool, crystallization;
Four, the white piperidine alcohols crystal above-mentioned crystallization hexanaphthene is washed, filtered refining.
Claims (1)
1. the preparation method of a tetramethyl--4-piperidine alcohols, is characterized in that: it comprises the following steps:
One, add in the autoclave with water-cooled tube, pressure warning unit, stirring, thermometer by piperidone, solvent, catalyzer, air three times in logical nitrogen replacement still, logical hydrogen, to 1MPa, stirs intensification 90 DEG C, reaction 1.4h;
Two, react complete, be cooled to 50 DEG C, emptying, take out material, leach catalyzer;
Three, gained filtrate is distilled, recycling design, remaining solution is carried out cool, crystallization;
Four, the white piperidine alcohols crystal above-mentioned crystallization hexanaphthene is washed, filtered refining.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310578374.7A CN104649957A (en) | 2013-11-19 | 2013-11-19 | 2,2,6,6-tetramethyl-4-pipradrol preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310578374.7A CN104649957A (en) | 2013-11-19 | 2013-11-19 | 2,2,6,6-tetramethyl-4-pipradrol preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104649957A true CN104649957A (en) | 2015-05-27 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310578374.7A Pending CN104649957A (en) | 2013-11-19 | 2013-11-19 | 2,2,6,6-tetramethyl-4-pipradrol preparation method |
Country Status (1)
| Country | Link |
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| CN (1) | CN104649957A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439940A (en) * | 2015-11-23 | 2016-03-30 | 宿迁市振兴化工有限公司 | Method for continuously producing triacetonamine with high stability by using melt crystallization technology |
| TWI738491B (en) * | 2020-09-03 | 2021-09-01 | 台灣中油股份有限公司 | Preparation method of tetramethylpiperidinol |
-
2013
- 2013-11-19 CN CN201310578374.7A patent/CN104649957A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439940A (en) * | 2015-11-23 | 2016-03-30 | 宿迁市振兴化工有限公司 | Method for continuously producing triacetonamine with high stability by using melt crystallization technology |
| CN105439940B (en) * | 2015-11-23 | 2018-03-09 | 宿迁市振兴化工有限公司 | A kind of method using fusion-crystallization technology continuous production high stability triacetonamine |
| TWI738491B (en) * | 2020-09-03 | 2021-09-01 | 台灣中油股份有限公司 | Preparation method of tetramethylpiperidinol |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150527 |
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| WD01 | Invention patent application deemed withdrawn after publication |