CN106478361A - The building-up process of bromoethane - Google Patents
The building-up process of bromoethane Download PDFInfo
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- CN106478361A CN106478361A CN201510535748.6A CN201510535748A CN106478361A CN 106478361 A CN106478361 A CN 106478361A CN 201510535748 A CN201510535748 A CN 201510535748A CN 106478361 A CN106478361 A CN 106478361A
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Abstract
The building-up process of bromoethane, including：In the round-bottomed flask of 100mL, add the finely ground sodium bromide of 6.5g, be then placed in 8ml water, vibration is allowed to dissolve.Add 5ml95% ethanol, under cooling and continuous shake, it is slowly added concentrated sulphuric acid, cool down flask with ice-water bath simultaneously, put into 2 ~ 3 zeolites again, add cold water and saturation sodium sulfite solution in accepter, be placed on cooling in ice-water bath, and so that the end connecing skirt has just been immersed in the aqueous solution of accepter.The flame using very little on asbestos gauge heats flask, and vial matter starts to foam, and controls flame size, so that oily mater is gradually distilled off, and distillation is milky grease, is sunken to bottom of bottle.
Description
Technical field
The present invention relates to the building-up process of bromoethane, belongs to synthesis chemical field.
Background technology
Bromoethane is the important source material of organic synthesiss.Agriculturally it is used as the fumigating insecticide in storage corn, warehouse and room etc..Bromoethane is to be formed with the sulphuric acid of freezing and ethanol synthesis by potassium bromide.It is usually used in the ethylization of gasoline, cryogen and anesthetis.Therefore, Chemical Manufacture workman and stifling work all can contact the bromoethane of variable concentrations.
In organic synthesiss, EtBr is imaginary ethyl carbonium ion（Et）Synthon.For example ethyl ester can will be converted into by carboxylate, carbanion to ethyl derivative, thiourea is to Ethyl isothiuronium salt, and amine is to ethylamine.Even if this liquid is present in room temperature, still very volatile.EtBr is commonly used for preparing alkaline Grignard reagent, and such as EtMgBr can make alkynes lose proton：EtBr + Mg → EtMgBr.
Content of the invention
The present invention provides the building-up process of bromoethane, including：In the round-bottomed flask of 100mL, add the finely ground sodium bromide of 6.5g, be then placed in 8ml water, vibration is allowed to dissolve.Add 5ml95% ethanol, under cooling and continuous shake, it is slowly added concentrated sulphuric acid, cool down flask with ice-water bath simultaneously, put into 2 ~ 3 zeolites again, add cold water and saturation sodium sulfite solution in accepter, be placed on cooling in ice-water bath, and so that the end connecing skirt has just been immersed in the aqueous solution of accepter.The flame using very little on asbestos gauge heats flask, and vial matter starts to foam, and controls flame size, so that oily mater is gradually distilled off, and distillation is milky grease, is sunken to bottom of bottle.Liquid in receptor is poured in separatory funnel, after stratification, the rough bromoethane of lower floor is put in dry fine taper bottle, conical flask is dipped in cooling in ice-water bath, gradually toward in bottle, adds concentrated sulphuric acid, vibrate simultaneously, the clear becoming until bromoethane, and bottom of bottle has liquid layer to separate（About need 2ml concentrated sulphuric acid）, carefully divide following sulfuric acid layer with the separatory funnel being dried, bromoethane layer poured into 30ml alembic from the suitable for reading of separatory funnel.
The invention has the beneficial effects as follows：The bromoethane of present invention preparation, preparation process is simply it is easy to operate.
Specific embodiment
Hereinafter the principle and feature of the present invention is described, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment 1
In the round-bottomed flask of 100mL, add the finely ground sodium bromide of 6.5g, be then placed in 8ml water, vibration is allowed to dissolve.Add 5ml95% ethanol, under cooling and continuous shake, it is slowly added concentrated sulphuric acid, cool down flask with ice-water bath simultaneously, put into 2 ~ 3 zeolites again, add cold water and saturation sodium sulfite solution in accepter, be placed on cooling in ice-water bath, and so that the end connecing skirt has just been immersed in the aqueous solution of accepter.The flame using very little on asbestos gauge heats flask, and vial matter starts to foam, and controls flame size, so that oily mater is gradually distilled off, and distillation is milky grease, is sunken to bottom of bottle.Liquid in receptor is poured in separatory funnel, after stratification, the rough bromoethane of lower floor is put in dry fine taper bottle, conical flask is dipped in cooling in ice-water bath, gradually toward in bottle, adds concentrated sulphuric acid, vibrate simultaneously, the clear becoming until bromoethane, and bottom of bottle has liquid layer to separate（About need 2ml concentrated sulphuric acid）, carefully divide following sulfuric acid layer with the separatory funnel being dried, bromoethane layer poured into 30ml alembic from the suitable for reading of separatory funnel, obtains 5 grams.
Embodiment 2
In the round-bottomed flask of 100mL, add the finely ground sodium bromide of 8g, be then placed in 10ml water, vibration is allowed to dissolve.Add 5ml95% ethanol, under cooling and continuous shake, it is slowly added concentrated sulphuric acid, cool down flask with ice-water bath simultaneously, put into 2 ~ 3 zeolites again, add cold water and saturation sodium sulfite solution in accepter, be placed on cooling in ice-water bath, and so that the end connecing skirt has just been immersed in the aqueous solution of accepter.The flame using very little on asbestos gauge heats flask, and vial matter starts to foam, and controls flame size, so that oily mater is gradually distilled off, and distillation is milky grease, is sunken to bottom of bottle.Liquid in receptor is poured in separatory funnel, after stratification, the rough bromoethane of lower floor is put in dry fine taper bottle, conical flask is dipped in cooling in ice-water bath, gradually toward in bottle, adds concentrated sulphuric acid, vibrate simultaneously, the clear becoming until bromoethane, and bottom of bottle has liquid layer to separate（About need 2ml concentrated sulphuric acid）, carefully divide following sulfuric acid layer with the separatory funnel being dried, bromoethane layer poured into 30ml alembic from the suitable for reading of separatory funnel, obtains 6 grams.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (2)
1. the building-up process of bromoethane, including：In the round-bottomed flask of 100mL，Add the finely ground sodium bromide of 6.5g，It is then placed in 8ml water，Vibration is allowed to dissolve，Add 5ml95% ethanol，Under cooling and continuous shake，It is slowly added concentrated sulphuric acid，Cool down flask with ice-water bath simultaneously，Put into 2 ~ 3 zeolites again，Cold water and saturation sodium sulfite solution is added in accepter，It is placed on cooling in ice-water bath，And so that the end connecing skirt has just been immersed in the aqueous solution of accepter，The flame using very little on asbestos gauge heats flask，Vial matter starts to foam，Control flame size，Oily mater is made gradually to be distilled off，Distillation is milky grease，It is sunken to bottom of bottle，Liquid in receptor is poured in separatory funnel，After stratification，The rough bromoethane of lower floor is put in dry fine taper bottle，Conical flask is dipped in cooling in ice-water bath，Toward in bottle, gradually add concentrated sulphuric acid，Vibrate simultaneously，The clear becoming until bromoethane，And bottom of bottle has liquid layer to separate，（About need 2ml concentrated sulphuric acid）, carefully divide following sulfuric acid layer with the separatory funnel being dried, bromoethane layer poured into 30ml alembic from the suitable for reading of separatory funnel.
2. the building-up process of bromoethane described in claim 1, the bromoethane being diverted in separatory funnel obtains pure bromoethane after needing rectification again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510535748.6A CN106478361A (en) | 2015-08-28 | 2015-08-28 | The building-up process of bromoethane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510535748.6A CN106478361A (en) | 2015-08-28 | 2015-08-28 | The building-up process of bromoethane |
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| CN106478361A true CN106478361A (en) | 2017-03-08 |
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| CN201510535748.6A Pending CN106478361A (en) | 2015-08-28 | 2015-08-28 | The building-up process of bromoethane |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467335A (en) * | 2018-05-30 | 2018-08-31 | 盐城市龙升化工有限公司 | The synthesis and production process of bromoethane |
| CN113666798A (en) * | 2021-07-16 | 2021-11-19 | 上虞新和成生物化工有限公司 | Green process for preparing bromoethane from bromine salt |
| CN114716480A (en) * | 2022-04-20 | 2022-07-08 | 黑龙江豪运药业有限公司 | Green synthesis method of n-propylphosphoric cyclic anhydride |
| CN113666798B (en) * | 2021-07-16 | 2024-06-04 | 上虞新和成生物化工有限公司 | Green technology for preparing bromoethane from bromate |
-
2015
- 2015-08-28 CN CN201510535748.6A patent/CN106478361A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467335A (en) * | 2018-05-30 | 2018-08-31 | 盐城市龙升化工有限公司 | The synthesis and production process of bromoethane |
| CN113666798A (en) * | 2021-07-16 | 2021-11-19 | 上虞新和成生物化工有限公司 | Green process for preparing bromoethane from bromine salt |
| CN113666798B (en) * | 2021-07-16 | 2024-06-04 | 上虞新和成生物化工有限公司 | Green technology for preparing bromoethane from bromate |
| CN114716480A (en) * | 2022-04-20 | 2022-07-08 | 黑龙江豪运药业有限公司 | Green synthesis method of n-propylphosphoric cyclic anhydride |
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Application publication date: 20170308 |
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