CN104713981A - Content calculation method of 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride generated by acylation reaction - Google Patents
Content calculation method of 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride generated by acylation reaction Download PDFInfo
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- CN104713981A CN104713981A CN201510130217.9A CN201510130217A CN104713981A CN 104713981 A CN104713981 A CN 104713981A CN 201510130217 A CN201510130217 A CN 201510130217A CN 104713981 A CN104713981 A CN 104713981A
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- fluorobenzoyl chloride
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Abstract
The invention discloses a content calculation method of 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride generated by acylation reaction. The content calculation method comprises a blank correction step, a sample measurement step and a calculation step. 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride can completely react with water to produce 2,4-dichloro-3-nitro-5-fluorobenzoic acid and HCl, and can completely react with methanol to produce 2,4-dichloro-3-nitro-5-methyl fluorobenzoate and HCl, and the specific content of 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride can be calculated according to the quantity of acid produced by the two reactions. The content calculation method of 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride generated by acylation reaction disclosed by the invention does not need to consider whether products can be influenced by moisture or not, is convenient and feasible to operate, ensures that both the time and labor can be saved, and is high in content calculation accuracy.
Description
Technical field
The present invention relates to a kind of cubage method that acylation reaction generates the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, belong to chemical reaction monitor and detection field.
Background technology
In 2,4-dichloro-3-nitro-5-fluorobenzoic acid and thionyl chloride (chlorating agent) course of reaction, how to measure benzoic acid and remain method a lot, the existence of NMR, infrared test carboxyl, gas chromatography test, n-hexane dissolution are tested.But having a shortcoming, is all the impact needing to avoid moisture on sample in test process, is all be difficult to avoid in real process, be difficult to determine whether to have carried out destruction due to ambient moisture to sample or actual sample is just not all right.
The present inventor finds, 2, the chloro-3-nitro of 4-bis--5-fluorobenzoyl chloride can by thoroughly reacting raw 2 with water, 4-dichloro-3-nitro-5-fluorobenzoic acid and HCl, generation 2,4-dichloro-3-nitro-5-fluorobenzoic acid methyl esters and HCl is thoroughly reacted, the amount of the acid generated by these two reactions with methyl alcohol, calculate the concrete content of 2,4-bis-chloro-3-nitro-5-fluorobenzoyl chloride.So just there is no need to consider whether whether moisture affect product.
Summary of the invention
The object of this invention is to provide a kind of cubage method that acylation reaction generates the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, to solve a still unsolved difficult problem in above-mentioned prior art.
The technical solution used in the present invention is: acylation reaction generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, and its innovative point is: comprise blank correction step, sample determination step and calculation procedure; Described blank correction step is that to take weight be W to precision
1sample 2,4-bis-chloro-3-nitro-5-fluorobenzoyl chloride, W
1=0.6 ± 0.04g, puts in the iodine flask filling 20ml methyl alcohol, jolting 60min, adds 3 phenolphthalein indicators, is titrated to pink with 0.5mol/L sodium hydroxide titration liquid, and the volume of consumption is V
1;
Described sample determination step is that to take weight be W to precision
2sample 2,4-bis-chloro-3-nitro-5-fluorobenzoyl chloride, W
2=0.6 ± 0.04g, puts in the iodine flask filling 5ml water, 15ml solvent, jolting 60min, adds 3 phenolphthalein indicators, be titrated to pink with 0.5mol/L sodium hydroxide titration liquid, and the volume of consumption is V
2.
Described calculation procedure is as follows:
In formula: the concentration mol/L of-----sodium hydroxide titration liquid
-----blank consumes the volume ml of NaOH
The quality g that-----is blank
-----sample consumes the volume ml of NaOH
The quality g of-----sample
Further, described iodine flask is 100ml iodine flask.
Further, described W
1and W
2quality be accurate to ten thousand/.
Further, the buret that described 0.5mol/L sodium hydroxide titration liquid uses is 50ml buret.
Further, described methyl alcohol is absolute methanol.
Further, in described sample determination step, solvent is dimethyl sulphoxide solution.
Beneficial effect: this acylation reaction of the present invention generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, there is no need to consider whether whether moisture affect product, and easy to operate feasible, time saving and energy saving, cubage accuracy is high.
Embodiment
Implementation column below can make those skilled in the art more fully understand the present invention, but does not therefore limit the present invention among described scope of embodiments.
embodiment 1
Blank correction step: precision takes sample 2, the 4-bis-chloro-3-nitro-5-fluorobenzoyl chloride that weight is W1, W
1=0.5892g, puts in the iodine flask filling 20ml methyl alcohol, jolting 60min, adds 3 phenolphthalein indicators, is titrated to pink with 0.4933mol/L sodium hydroxide titration liquid, and the volume of consumption is V
14.36ml
Sample determination step: precision takes the sample 2 that weight is W2, the chloro-3-nitro of 4-bis--5-fluorobenzoyl chloride, W2=0.5989g, put in the iodine flask filling 5ml water, 15ml solvent, jolting 60min, add 3 phenolphthalein indicators, be titrated to pink with 0.4933mol/L sodium hydroxide titration liquid, the volume of consumption is V
2=8.88 ml.
Cubage:
=99.8
embodiment 2
Blank correction step: it is W that precision takes weight
1sample 2,4-bis-chloro-3-nitro-5-fluorobenzoyl chloride, W
1=0.6121g, puts in the iodine flask filling 20ml methyl alcohol, jolting 60min, adds 3 phenolphthalein indicators, is titrated to pink with 0.4998mol/L sodium hydroxide titration liquid, and the volume of consumption is V
1=4.50 ml
Sample determination step: precision takes sample 2, the 4-bis-chloro-3-nitro-5-fluorobenzoyl chloride that weight is W2, W
2=0.6011g, puts in the iodine flask filling 5ml water, 15ml solvent, jolting 60min, adds 3 phenolphthalein indicators, be titrated to pink with 0.4998mol/L sodium hydroxide titration liquid, and the volume of consumption is V
2=8.82 ml.
Cubage
=99.7。
Claims (6)
1. acylation reaction generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, it is characterized in that: comprise blank correction step, sample determination step and calculation procedure; Described blank correction step is that to take weight be W to precision
1sample 2,4-bis-chloro-3-nitro-5-fluorobenzoyl chloride, W1=0.6 ± 0.04g, puts in the iodine flask filling 20ml methyl alcohol, jolting 60min, adds 3 phenolphthalein indicators, is titrated to pink with 0.5mol/L sodium hydroxide titration liquid, and the volume of consumption is V
1;
Described sample determination step is that to take weight be W to precision
2sample 2,4-bis-chloro-3-nitro-5-fluorobenzoyl chloride, W
2=0.6 ± 0.04g, puts in the iodine flask filling 5ml water, 15ml solvent, jolting 60min, adds 3 phenolphthalein indicators, be titrated to pink with 0.5mol/L sodium hydroxide titration liquid, and the volume of consumption is V
2.
2. described in, calculation procedure is as follows:
In formula: the concentration mol/L of-----sodium hydroxide titration liquid
-----blank consumes the volume ml of NaOH
The quality g that-----is blank
-----sample consumes the volume ml of NaOH
The quality g of-----sample
Acylation reaction according to claim 1 generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, it is characterized in that: described iodine flask is 100ml iodine flask.
3. acylation reaction according to claim 1 generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, it is characterized in that: described W
1and W
2quality be accurate to ten thousand/.
4. acylation reaction according to claim 1 generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, it is characterized in that: the buret that described 0.5mol/L sodium hydroxide titration liquid uses is 50ml buret.
5. acylation reaction according to claim 1 generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, it is characterized in that: described methyl alcohol is absolute methanol.
6. acylation reaction according to claim 1 generates the cubage method of the chloro-3-nitro of 2,4-bis--5-fluorobenzoyl chloride, it is characterized in that: in described sample determination step, solvent is dimethyl sulphoxide solution.
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|---|---|---|---|
| CN201510130217.9A CN104713981A (en) | 2014-05-21 | 2015-03-24 | Content calculation method of 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride generated by acylation reaction |
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| CN2014102157286 | 2014-05-21 | ||
| CN201410215728 | 2014-05-21 | ||
| CN201510130217.9A CN104713981A (en) | 2014-05-21 | 2015-03-24 | Content calculation method of 2,4-dichloro-3-nitro-5-fluorobenzoyl chloride generated by acylation reaction |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070135610A1 (en) * | 2005-12-09 | 2007-06-14 | General Electric Company | Polyarylate acid chloride compositions and derivatives therefrom |
| EP1971646A1 (en) * | 2005-12-09 | 2008-09-24 | General Electric Company | Polyarylate compositions useful as coatings , their preparation, and articles made therefrom |
| CN101723923A (en) * | 2009-12-15 | 2010-06-09 | 上海师范大学 | N-2, 4-dichlorophenoxy acetyl (sulfur) carbamide weedicide and preparation method thereof |
-
2015
- 2015-03-24 CN CN201510130217.9A patent/CN104713981A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070135610A1 (en) * | 2005-12-09 | 2007-06-14 | General Electric Company | Polyarylate acid chloride compositions and derivatives therefrom |
| EP1971646A1 (en) * | 2005-12-09 | 2008-09-24 | General Electric Company | Polyarylate compositions useful as coatings , their preparation, and articles made therefrom |
| CN101723923A (en) * | 2009-12-15 | 2010-06-09 | 上海师范大学 | N-2, 4-dichlorophenoxy acetyl (sulfur) carbamide weedicide and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 司捷: "电位滴定法测定草酰氯含量", 《辽宁化工》 * |
| 王艳 等: "阿洛西林合成中间体咪唑酰氯含量的测定", 《理化检验-化学分册》 * |
| 谢淼: "卡尔弗休试剂测定乙酸氯的含量", 《医药工业》 * |
| 魏天俊等: "工业氯乙酰氯含量的测定", 《中国医药工业杂志》 * |
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