CN106673954A - Preparation method of diiodomethane - Google Patents
Preparation method of diiodomethane Download PDFInfo
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- CN106673954A CN106673954A CN201510745591.XA CN201510745591A CN106673954A CN 106673954 A CN106673954 A CN 106673954A CN 201510745591 A CN201510745591 A CN 201510745591A CN 106673954 A CN106673954 A CN 106673954A
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- diiodomethane
- preparation
- sodium iodide
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- dichloromethane
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Abstract
The invention discloses a preparation method of diiodomethane. The preparation method is characterized by comprising the following steps: synthesizing diiodomethane, washing, and refining. The preparation method has the advantages that by reasonably adjusting the production process, the process operation is simple, the yield of products is increased, the market requirement can be met, and the economic benefit and social benefit of enterprises can be improved.
Description
Technical field
The invention belongs to organic compound preparation method field, and in particular to a kind of preparation method of diiodomethane.
Background technology
Diiodomethane, molecular formula is CH2I2, and molecular weight is 267.87, and achromaticity and clarification, as analytical reagent, is also used for organic synthesiss to faint yellow heavy liquid；One of domestic and international bulk article, be widely used in organic synthesiss, the analysis of mineral and separate, the measure of the identification of pyridine and coefficient of refraction, be especially largely used to synthesis cyclopropane.At present, in the case where not increasing sophisticated equipment and not increasing operator's technical requirements, the product yield for synthesizing is not high.
The content of the invention
Present invention aims to the deficiencies in the prior art, now provide a kind of process is simple, the preparation method of the high diiodomethane of synthesis yield.
For achieving the above object, the technical scheme is that：A kind of preparation method of diiodomethane, its innovative point is：The preparation of diiodomethane is completed including diiodomethane synthetic reaction, washing and purification step, is comprised the following steps that：
（1）Diiodomethane synthetic reaction
Ratio of weight and number by the mixing of sodium iodide, dichloromethane and solvent dimethylformamide, sodium iodide and dichloromethane is 3: 1, and sodium iodide and dimethylformamide ratio of weight and number are 1: 1.5-1.7, are stirred and heated to 90 DEG C, isothermal reaction 4-8 hours；
（2）Washing
A, into reacted mixture hypo solution is added, stirred, stratification discards water layer；
B, addition clear water, stir, and stratification discards water layer；
（3）It is refined
Vacuum distillation, obtains diiodomethane finished product.
Beneficial effects of the present invention are as follows：The present invention passes through Reasonable adjustment production technology so that technological operation is simple, and improves product yield, meets the demand in market, improves the economic benefit and social benefit of enterprise.
Specific embodiment
Hereinafter embodiments of the present invention are illustrated by particular specific embodiment, the content that those skilled in the art can be by disclosed by this specification understands easily other advantages and effect of the present invention.
Embodiment 1
A kind of preparation method of diiodomethane, including diiodomethane synthetic reaction, washing and purification step complete the preparation of diiodomethane, comprises the following steps that：
（1）Diiodomethane synthetic reaction
Ratio of weight and number by the mixing of sodium iodide, dichloromethane and solvent dimethylformamide, sodium iodide and dichloromethane is 3: 1, and sodium iodide and dimethylformamide ratio of weight and number are 1: 1.5, are stirred and heated to 90 DEG C, isothermal reaction 4 hours；
（2）Washing
A, into reacted mixture hypo solution is added, stirred, stratification discards water layer；
B, addition clear water, stir, and stratification discards water layer；
（3）It is refined
Vacuum distillation, obtains diiodomethane finished product.
Embodiment 2
A kind of preparation method of diiodomethane, including diiodomethane synthetic reaction, washing and purification step complete the preparation of diiodomethane, comprises the following steps that：
（1）Diiodomethane synthetic reaction
Ratio of weight and number by the mixing of sodium iodide, dichloromethane and solvent dimethylformamide, sodium iodide and dichloromethane is 3: 1, and sodium iodide and dimethylformamide ratio of weight and number are 1: 1.7, are stirred and heated to 90 DEG C, isothermal reaction 8 hours；
（2）Washing
A, into reacted mixture hypo solution is added, stirred, stratification discards water layer；
B, addition clear water, stir, and stratification discards water layer；
（3）It is refined
Vacuum distillation, obtains diiodomethane finished product.
Embodiment 3
A kind of preparation method of diiodomethane, including diiodomethane synthetic reaction, washing and purification step complete the preparation of diiodomethane, comprises the following steps that：
（1）Diiodomethane synthetic reaction
Ratio of weight and number by the mixing of sodium iodide, dichloromethane and solvent dimethylformamide, sodium iodide and dichloromethane is 3: 1, and sodium iodide and dimethylformamide ratio of weight and number are 1: 1.6, are stirred and heated to 90 DEG C, isothermal reaction 6 hours；
（2）Washing
A, into reacted mixture hypo solution is added, stirred, stratification discards water layer；
B, addition clear water, stir, and stratification discards water layer；
（3）It is refined
Vacuum distillation, obtains diiodomethane finished product.
The present invention passes through Reasonable adjustment production technology so that technological operation is simple, and improves product yield, meets the demand in market, improves the economic benefit and social benefit of enterprise.
Above-described embodiment is presently preferred embodiments of the present invention; it is not the restriction to technical solution of the present invention; as long as without the technical scheme that creative work can be realized on the basis of above-described embodiment, in the rights protection scope for being regarded as falling into patent of the present invention.
Claims (1)
1. a kind of preparation method of diiodomethane, it is characterised in that：The preparation of diiodomethane is completed including diiodomethane synthetic reaction, washing and purification step, is comprised the following steps that：
（1）Diiodomethane synthetic reaction
Ratio of weight and number by the mixing of sodium iodide, dichloromethane and solvent dimethylformamide, sodium iodide and dichloromethane is 3: 1, and sodium iodide and dimethylformamide ratio of weight and number are 1: 1.5-1.7, are stirred and heated to 90 DEG C, isothermal reaction 4-8 hours；
（2）Washing
A, into reacted mixture hypo solution is added, stirred, stratification discards water layer；
B, addition clear water, stir, and stratification discards water layer；
（3）It is refined
Vacuum distillation, obtains diiodomethane finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510745591.XA CN106673954A (en) | 2015-11-06 | 2015-11-06 | Preparation method of diiodomethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510745591.XA CN106673954A (en) | 2015-11-06 | 2015-11-06 | Preparation method of diiodomethane |
Publications (1)
| Publication Number | Publication Date |
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| CN106673954A true CN106673954A (en) | 2017-05-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201510745591.XA Pending CN106673954A (en) | 2015-11-06 | 2015-11-06 | Preparation method of diiodomethane |
Country Status (1)
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| CN (1) | CN106673954A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501037A (en) * | 2017-09-08 | 2017-12-22 | 南通意特化工有限公司 | A kind of preparation method of diiodomethane |
| CN112961029A (en) * | 2021-02-02 | 2021-06-15 | 浙江肯特催化材料科技有限公司 | Preparation method of diiodomethane |
-
2015
- 2015-11-06 CN CN201510745591.XA patent/CN106673954A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501037A (en) * | 2017-09-08 | 2017-12-22 | 南通意特化工有限公司 | A kind of preparation method of diiodomethane |
| CN112961029A (en) * | 2021-02-02 | 2021-06-15 | 浙江肯特催化材料科技有限公司 | Preparation method of diiodomethane |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170517 |