CN1250043A - Resin catalysis to synthesize folic acetate - Google Patents
Resin catalysis to synthesize folic acetate Download PDFInfo
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- CN1250043A CN1250043A CN 98121503 CN98121503A CN1250043A CN 1250043 A CN1250043 A CN 1250043A CN 98121503 CN98121503 CN 98121503 CN 98121503 A CN98121503 A CN 98121503A CN 1250043 A CN1250043 A CN 1250043A
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- reaction
- ion exchange
- exchange resin
- acetate
- resin
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The present invention uses ion exchange resin as catalyst. Acetic acid, cis-3-hexen-1-ol and ion exchange resin are mixed in certain proportion, and the mixture is heated and stirred with the reaction period being controlled. After the reaction is finished and through filtering to eliminate ion exchange resin, neutralization, water washing, drying and distillation or depression distillation, folic ester acetate is collected. The said technological process has simple reaction, less side product and simple post-reaction treatment and the resin may be reused.
Description
The present invention relates to a kind of chemical spices.
Verdural extensively is present in the plants such as fruit, flower and tealeaves, is a kind of widely used perfume material.China's approved uses.People's diacetyl oxide commonly used and leaf-alcohol react and prepare verdural and (see Bohnsack, Chem.Ber., 75,74,1942), though productive rate can reach 75%, but the price of diacetyl oxide is more than 4 times of acetate, and reaction simultaneously also will add a certain amount of sodium acetate, has improved the cost of raw material.People utilized catalyzed reaction to prepare acetate leaf-alcohol [Yoshida, Yoshinori, et.al:Japan Kokai 7717,411 (C1.C07C69/145), 09 Feb 1977, Appl.75/93,193,01 Aug 1975 from positive amylene again afterwards; 4pp], productive rate is 56%.But this reaction process more complicated, and product separation is not easy, and also can influence the quality of product.
The objective of the invention is to overcome above-mentioned weak point, simplify Production Flow Chart and post-reaction treatment, reduced raw materials cost, catalyzer can be recycled, and reduces the generation of the three wastes, helps keeping ecotope.
The technical scheme of realization the object of the invention is made up of following four steps:
With acetate, leaf-alcohol and ion exchange resin by weight (1.2-5.0): 1: (0.50-1.00) join in the round-bottomed flask, heating, controlled temperature stirs, in 2 hours reaction times at 70-120 ℃.Reaction formula is as follows:
2. reaction is finished, and removes by filter ion exchange resin, and filtrate water is washed, and with the aqueous sodium carbonate neutralization, the water reaction is washed till neutrality more again.
3. use the anhydrous sodium sulfate drying organic phase, distill again at last or underpressure distillation collection product.The verdural yield is up to more than 65%.
4. clean ion exchange resin, this resin can use repeatedly.Beneficial effect of the present invention is as follows:
React relatively simple, by product is few.Simple as reaction raw materials, have only acetate and leaf-alcohol, conversion unit is simple.The aftertreatment of reaction is also very simple, as long as resin filter is removed, can obtain product with back redistillation or underpressure distillation in the filtrate.Also can make the reaction serialization by column reactor.
Embodiment:
Add leaf-alcohol 10.0g in the 50ml two-mouth bottle, glacial acetic acid 12.0g (0.2mol), ion exchange resin 7.5g stirs, and is heated to 110 ℃, coreaction 2 hours.Be chilled to room temperature after the reaction, remove by filter resin, filtrate is through gas chromatographic analysis, and its transformation efficiency is 69%.Filtrate is through washing, and the sodium carbonate solution neutralization is washed to neutrality.Again through anhydrous sodium sulfate drying, through distill verdural 6.6g.
Claims (1)
1. resin catalysis to synthesize folic acetate is characterized in that: it is intact as follows that spent ion exchange resin is made catalyzer:
(1) with acetate, leaf-alcohol and ion exchange resin by weight (1.2-5.0): 1; (0.5-1.0) join in the round-bottomed flask, heating, controlled temperature stirs at 70-120 ℃, and the reaction times is in 2 hours.Reaction formula is as follows:
(2) reaction is finished, and removes by filter ion exchange resin, and filtrate water is washed, and with the aqueous sodium carbonate neutralization, is being washed to neutrality again.
(3) use the anhydrous sodium sulfate drying organic phase, distill, collect product, the verdural yield is up to 65%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98121503A CN1122016C (en) | 1998-10-05 | 1998-10-05 | Resin catalysis to synthesize folic acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98121503A CN1122016C (en) | 1998-10-05 | 1998-10-05 | Resin catalysis to synthesize folic acetate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250043A true CN1250043A (en) | 2000-04-12 |
| CN1122016C CN1122016C (en) | 2003-09-24 |
Family
ID=5227129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98121503A Expired - Fee Related CN1122016C (en) | 1998-10-05 | 1998-10-05 | Resin catalysis to synthesize folic acetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1122016C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420832A (en) * | 2013-09-04 | 2013-12-04 | 天宁香料（江苏）有限公司 | Preparing method of cis-3-Hexenyl caproate |
| CN111807957A (en) * | 2020-07-02 | 2020-10-23 | 深圳飞扬兴业科技有限公司 | Synthetic method of geranyl acetate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5217411A (en) * | 1975-08-01 | 1977-02-09 | Japan Synthetic Rubber Co Ltd | Process for preparation of unsaturated primary alcohol esters |
-
1998
- 1998-10-05 CN CN98121503A patent/CN1122016C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420832A (en) * | 2013-09-04 | 2013-12-04 | 天宁香料（江苏）有限公司 | Preparing method of cis-3-Hexenyl caproate |
| CN111807957A (en) * | 2020-07-02 | 2020-10-23 | 深圳飞扬兴业科技有限公司 | Synthetic method of geranyl acetate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1122016C (en) | 2003-09-24 |
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