CN102503835A - Synthetic method for ammonium salt - Google Patents
Synthetic method for ammonium salt Download PDFInfo
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- CN102503835A CN102503835A CN2011103602108A CN201110360210A CN102503835A CN 102503835 A CN102503835 A CN 102503835A CN 2011103602108 A CN2011103602108 A CN 2011103602108A CN 201110360210 A CN201110360210 A CN 201110360210A CN 102503835 A CN102503835 A CN 102503835A
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- xylene diamine
- diamine dihydrochloride
- ammonium salt
- meta
- synthetic method
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Abstract
The invention discloses a synthetic method for meta-xylylene diamine dihydrochloride. The method comprises the following steps of: reacting meta-xylylene diamine with manganese chloride tetrahydrate in the ratio of 2:1 in an absolute ethyl alcohol solution for one day; thermally filtering a reaction liquid; dissolving with ethanol; screwing a half of a solvent out; standing for certain days; and precipitating white meta-xylylene diamine dihydrochloride crystals out.
Description
One, technical field
The present invention relates to a kind of preparation and compound method of ammonium salt, exactly is a kind of preparation and compound method of m-xylene diamine dihydrochloride.
Two, background technology
The compound method of ammonium salt has many bibliographical informations.As far back as 1956, J.Chem.Soc. reported the compound method of some ammonium salts, and nineteen fifty-nine, J.Am.Chem.Soc. has also reported the compound method of ammonium salt class.(1.Surrey，Alexander?R.；Lesher，George?Y.；Mayer，J.Richard；Webb，Wm.G.Journal?of?the?American?Chemical?Society(1959)，81?2894-7；2.Davis，M.Journal?of?the?Chemical?Society(1956)，337-43.)。
The applicant does not obtain the title product title complex in the experiment of synthetic m-xylene diamine and four hydration hydration Manganous chloride tetrahydrate title complexs, but obtained another kind of novel cpd m-xylene diamine dihydrochloride.
Three, summary of the invention
The present invention aims to provide compound m-xylene diamine dihydrochloride, and technical problem to be solved is that one-step synthesis obtains title product.
The alleged a kind of m-xylene diamine dihydrochloride of the present invention be by the preparation of m-xylene diamine and four hydration Manganous chloride tetrahydrates by the compound shown in the following chemical formula:
Chemical name: the m-xylene diamine dihydrochloride, be called for short compound (I).
This compound method comprises synthetic and separates described Synthetic 2: 1 m-xylene diamine and four hydration Manganous chloride tetrahydrates reacted in ethanol solution one day, with the reaction solution heat filtering, react end after, filtered while hot obtains flaxen filtrating.Directly revolve driedly to filtrating, behind dissolve with ethanol, revolve half solvent again, leave standstill, have crystal to separate out after a couple of days.
This reaction mechanism can infer for the amino reactive hydrogen in the m-xylene diamine molecule and cl ions under the effect of alcohol solvent, form hydrochloric acid rapidly, and become ammonium salt with m-xylene diamine.
One step of this compound method obtains title product, and technology is simple, and is easy to operate.
Four, description of drawings
Fig. 1 is the X-diffraction analysis figure of m-xylene diamine dihydrochloride.
Five, embodiment
1. the preparation of m-xylene diamine dihydrochloride
Measure 1.6mL (about 0.012mol) m-xylene diamine and put into the 100mL round-bottomed flask, add the 30mL absolute ethyl alcohol, stir and make its dissolving; With 1.2327g (0.006mol) MnCl
24H
2O adds above-mentioned solution, heated and stirred backflow 24h; After reaction finished, filtered while hot obtained flaxen filtrating.Directly revolve driedly to filtrating, behind dissolve with ethanol, revolve half solvent again, leave standstill, have crystal to separate out after a couple of days.Product 0.4182g, productive rate 33%, fusing point: 124 ℃; Infrared data (KBr compressing tablet): 3309,2941,2626,2158,1601,1491,1375,1022,930,784,701; Ultimate analysis: C, 47.93; H, 6.86; N, 13.47.
Claims (1)
1. the compound method of a m-xylene diamine dihydrochloride; Comprise and synthesize and separate, it is characterized in that 2.: 1 m-xylene diamine and four hydration Manganous chloride tetrahydrates reacted one day in ethanol solution, the reaction solution heat filtering; Behind dissolve with ethanol; Revolve half solvent again, leave standstill, have crystal white m-xylene diamine dihydrochloride to separate out after a couple of days.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103602108A CN102503835A (en) | 2011-11-14 | 2011-11-14 | Synthetic method for ammonium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103602108A CN102503835A (en) | 2011-11-14 | 2011-11-14 | Synthetic method for ammonium salt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102503835A true CN102503835A (en) | 2012-06-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011103602108A Pending CN102503835A (en) | 2011-11-14 | 2011-11-14 | Synthetic method for ammonium salt |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1003219B (en) * | 1955-04-16 | 1957-02-28 | Bayer Ag | Process for the preparation of bis (aminomethyl) arylenes |
| CN1341096A (en) * | 1999-12-14 | 2002-03-20 | 昭和电工株式会社 | Process for producing of cyanobenzyamine of derivative |
| CN1931834A (en) * | 2005-09-13 | 2007-03-21 | 杭州崇舜化学有限公司 | Synthesis process of phenyl dimethylene diisocyanate |
| CN101973891A (en) * | 2010-11-04 | 2011-02-16 | 罗梅 | Preparation of chiral (S)-alpha-phenylethylamine hydrochloride and synthesis method thereof |
| CN102206159A (en) * | 2011-03-22 | 2011-10-05 | 罗梅 | Preparation method and synthesizing method of alpha-phenylethylamine acetate |
-
2011
- 2011-11-14 CN CN2011103602108A patent/CN102503835A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1003219B (en) * | 1955-04-16 | 1957-02-28 | Bayer Ag | Process for the preparation of bis (aminomethyl) arylenes |
| CN1341096A (en) * | 1999-12-14 | 2002-03-20 | 昭和电工株式会社 | Process for producing of cyanobenzyamine of derivative |
| CN1931834A (en) * | 2005-09-13 | 2007-03-21 | 杭州崇舜化学有限公司 | Synthesis process of phenyl dimethylene diisocyanate |
| CN101973891A (en) * | 2010-11-04 | 2011-02-16 | 罗梅 | Preparation of chiral (S)-alpha-phenylethylamine hydrochloride and synthesis method thereof |
| CN102206159A (en) * | 2011-03-22 | 2011-10-05 | 罗梅 | Preparation method and synthesizing method of alpha-phenylethylamine acetate |
Non-Patent Citations (1)
| Title |
|---|
| HUA CHENG，HUISHENG LI: "(m-Phenylenedimethylene)diammonium dichloride", 《ACTA CRYSTALLOGRAPHICA SECTION E》, vol. 64, 30 November 2008 (2008-11-30), pages 1 * |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120620 |