CN102234252A - Preparation method of bioregulator folcisteine - Google Patents
Preparation method of bioregulator folcisteine Download PDFInfo
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- CN102234252A CN102234252A CN2010101662947A CN201010166294A CN102234252A CN 102234252 A CN102234252 A CN 102234252A CN 2010101662947 A CN2010101662947 A CN 2010101662947A CN 201010166294 A CN201010166294 A CN 201010166294A CN 102234252 A CN102234252 A CN 102234252A
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- foline
- biological regulator
- formaldehyde
- yield
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
Abstract
The invention aims at overcoming the shortcomings of the prior art and provides a high-yield preparation method of folcisteine. The high-yield preparation method of folcisteine provided by the invention comprises the following steps: reacting cysteine (hydrochloride) and formaldehyde (paraformaldehyde), and then carrying out acetylation reaction (with acetic anhydride or acetyl chloride) to obtain a high-yield finished product. The preparation method has the beneficial effects of wide sources of raw materials, simple preparation method, easy operation process and high product yield, and the folcisteine can increase the yield of wheat, rice, corn, apples and other crops, and is used in the agricultural field.
Description
[technical field]
The present invention relates to the preparation method of a kind of half foline [3-ethanoyl-4-Thiazolidinecarboxylacid acid].
[background technology]
Half foline, English name Folcisteine, another name 3-Acetylthiazolidine-4-carboxylicacid chemical name: 3-ethanoyl-4-Thiazolidinecarboxylacid acid, N-acetyl thio proline(Pro).
Half foline is a kind of experimental biostimulation growth regulator, effective object and using method: increase the output to wheat, paddy rice, corn, apple and some other crops.Can be used for promoting the growth of seed germination and crop, improving fruit tree fruit-setting rate and amount of application is 0.25～0.5ml (effective constituent)/L.
The method of preparation half foline involved in the present invention, the productive rate height, easy and simple to handle.
[summary of the invention]
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method of produced in high yields half foline is provided.The method of synthetic half foline of high yield involved in the present invention: with halfcystine (hydrochloride) and formaldehyde (Paraformaldehyde 96) effect, carry out acetylizad reaction (using diacetyl oxide or Acetyl Chloride 98Min.) then and generate, obtain the finished product of high yield.
It is characterized in that processing step is:
Step 1 is mixed halfcystine, mineral alkali, formaldehyde, stirring at room, and 1～3h reaction is finished.
Step 2, room temperature leaves standstill, suction filtration.
Step 3, vacuum-drying obtains intermediate 4-Thiazolidinecarboxylacid acid.
Step 4 is with 4-Thiazolidinecarboxylacid acid and acetylation reagent reaction, temperature rising reflux.
Step 5 concentrates, washing, and vacuum-drying obtains the final product of high yield.
In the step 1, described formaldehyde mixed solution is that formaldehyde is 37% formalin.
In the step 3, described vacuum-drying is 50～80 ℃ of constant temperature 2～4h of temperature.
In the step 4, acetylation reagent relates to diacetyl oxide, and Acetyl Chloride 98Min. etc. preferentially use diacetyl oxide.
In the step 4, described return time is 0.5～3h.
In the step 5, described vacuum drying temperature is 50～80 ℃ of following constant temperature 1～4h.
The present invention has following beneficial effect: raw material sources are extensive, and the preparation method is simple, and are easy to operate, and produced in high yields obtains product.
[embodiment]
The invention will be further described below in conjunction with embodiment.Production technology of the present invention is to implement easily to this professional people.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment
In the 250ml round-bottomed flask, add the 20g cysteine hydrochloride, the 11.4g anhydrous sodium acetate, water and alcohol mixeding liquid (96ml, 1: 1, v/v), 42.8ml 37% formaldehyde solution, stirring at room 1 hour leaves standstill, and suction filtration gets thick product, oven dry, product is a white crystal, productive rate: 91%, and product is directly used in next step reaction.
In the 250ml round-bottomed flask, add 20g 4-Thiazolidinecarboxylacid acid, 60ml water, stir, add the 60ml diacetyl oxide, reflux 1h, be cooled to room temperature, frozen water cooling, enriched product, add 60ml water to residue, separate out white solid, suction filtration, wash product with water, vacuum-drying, 60 ℃ of freeze-day with constant temperature 2h, weigh productive rate 90%, mp:145-146C.
Utilize aforesaid method can make half foline of high yield, and reach its distinctive beneficial effect.
Claims (6)
1. the present invention is a kind of preparation method of biological regulator half foline, comprises the steps:
Step 1 is mixed halfcystine, mineral alkali, formaldehyde, stirring at room, and 1～3h reaction is finished.
Step 2, room temperature leaves standstill, suction filtration.
Step 3, vacuum-drying obtains intermediate 4-Thiazolidinecarboxylacid acid.
Step 4 is with 4-Thiazolidinecarboxylacid acid and acetylation reagent reaction, temperature rising reflux.
Step 5 concentrates, washing, and vacuum-drying obtains the final product of high yield.
2. the preparation method of a kind of biological regulator half foline according to claim 1 is characterized in that in the step 1, and described formaldehyde mixed solution is that formaldehyde is 37% formalin.
3. the preparation method of a kind of biological regulator half foline according to claim 1 is characterized in that in the step 3, and described vacuum-drying is 50～80 ℃ of constant temperature 2～4h of temperature.
4. the preparation method of a kind of biological regulator half foline according to claim 1 is characterized in that in the step 4, acetylation reagent relates to diacetyl oxide, and Acetyl Chloride 98Min. etc. preferentially use diacetyl oxide.
5. the preparation method of a kind of biological regulator half foline according to claim 1 is characterized in that in the step 4, and described return time is 0.5～3h.
6. the preparation method of a kind of biological regulator half foline according to claim 1 is characterized in that in the step 5, and described vacuum drying temperature is 50～80 ℃ of following constant temperature 1～4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101662947A CN102234252A (en) | 2010-05-05 | 2010-05-05 | Preparation method of bioregulator folcisteine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101662947A CN102234252A (en) | 2010-05-05 | 2010-05-05 | Preparation method of bioregulator folcisteine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102234252A true CN102234252A (en) | 2011-11-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101662947A Pending CN102234252A (en) | 2010-05-05 | 2010-05-05 | Preparation method of bioregulator folcisteine |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592083A (en) * | 2015-01-06 | 2015-05-06 | 宁波海硕生物科技有限公司 | Method for preparing N-acetyl-DL-thioproline |
| CN106386816A (en) * | 2016-08-31 | 2017-02-15 | 四川龙蟒福生科技有限责任公司 | Composition, preparation and application thereof |
| CN109053622A (en) * | 2018-09-05 | 2018-12-21 | 成都百事兴科技实业有限公司 | A kind of synthetic method of half foline of efficient preparation |
| CN111377879A (en) * | 2020-04-14 | 2020-07-07 | 苏州敬业医药化工有限公司 | Preparation method of L-thiazolidine-4-formic acid |
-
2010
- 2010-05-05 CN CN2010101662947A patent/CN102234252A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592083A (en) * | 2015-01-06 | 2015-05-06 | 宁波海硕生物科技有限公司 | Method for preparing N-acetyl-DL-thioproline |
| CN106386816A (en) * | 2016-08-31 | 2017-02-15 | 四川龙蟒福生科技有限责任公司 | Composition, preparation and application thereof |
| CN106386816B (en) * | 2016-08-31 | 2019-03-22 | 四川龙蟒福生科技有限责任公司 | A kind of composition, preparation and its application |
| CN109053622A (en) * | 2018-09-05 | 2018-12-21 | 成都百事兴科技实业有限公司 | A kind of synthetic method of half foline of efficient preparation |
| CN111377879A (en) * | 2020-04-14 | 2020-07-07 | 苏州敬业医药化工有限公司 | Preparation method of L-thiazolidine-4-formic acid |
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| C06 | Publication | ||
| PB01 | Publication | ||
| DD01 | Delivery of document by public notice |
Addressee: Zhang Yongchang Document name: Notification of Publication of the Application for Invention |
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| DD01 | Delivery of document by public notice |
Addressee: Zhang Yongchang Document name: Notification of before Expiration of Request of Examination as to Substance |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111109 |