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Generation of phosphorus oxychloride as by-product from phosphorus pentachloride and dmf and its use for chlorination reaction by converting into vilsmeier-haack reagent.

A technology for by-products and reagents, which is used in the production of by-product phosphorus oxychloride from phosphorus pentachloride and DMF and its application in the chlorination reaction by converting it into VILSMEIER-HAACK reagent

Inactive Publication Date: 2009-07-22
V B MEDICARE PVT LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] Therefore, all prior art references are limited to using PCl 5 Generation of Vilsmeier's reagent and use of this Vilsmeier's reagent in the form of DMF-insoluble solid crystals

Method used

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  • Generation of phosphorus oxychloride as by-product from phosphorus pentachloride and dmf and its use for chlorination reaction by converting into vilsmeier-haack reagent.

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1, after forming the first batch of Vilsmeier-Haack reagents, using 5 By-product POCl formed 3 Formation of the second batch of Vilsmeier-Haack reagents

[0034] At 20°C, 835g of PCl 5 Add to a round bottom flask containing 0.835L DMF. The completion of the Vilsmeier-Haack reaction was indicated by the formation of white crystals of the Vilsmeier-Haack reagent. After about 15 minutes, the generated POCl 3 Vilsmeier-Haack reagent also started to form and an orange-red solution formed with the solid. The mixture was then stirred thoroughly at room temperature for 1.0 hour. A 500ml excess of DMF was added to the reaction. The mixture was cooled to 0°C and a substrate containing 263 g of sucrose equivalent (sucrose-6-acetate) was added dropwise. The temperature was kept below 0°C during the dropwise addition.

[0035] After the substrate addition was complete, the temperature was allowed to come to room temperature and stirred for 1.0 hour. The temperature ...

Embodiment 2

[0036] Embodiment 2, utilize only by PCl 5 Chlorination of the formed Vilsmeier-Haack reagent

[0037] This experiment was performed to show that using only PCl 5 Efficiency of the chlorination reaction of the resulting Vilsmeier-Haack reagent. At 20°C, 835g of PCl 5 Add to a round bottom flask containing 0.835L DMF. The Vilsmeier-Haack reaction was complete and the formation of white crystals of the Vilsmeier-Haack reagent was observed. The reaction simultaneously forms POCl 3 , the POCl 3 Start the reaction with excess DMF to form the second Vilsmeier-Haack reagent. But the formed Vilsmeier-Haack reagent is in liquid form and does not become as in PCl 5 The solid Vilsmeier-Haack reagent in the reaction. Therefore, in order to determine and prove that by PCl 5 Efficiency of the formed Vilsmeier-Haack reagent, filtering off the formed PCl 5 Vilsmeier-Haack reagent, POCl 3 and excess DMF were thoroughly separated. The solid form of the Vilsmeier-Haack reagent was wa...

Embodiment 3

[0040] Embodiment 3, utilize only by POCl 3 Chlorination of the formed Vilsmeier-Haack reagent

[0041] This experiment was performed to show that using only POCl 3 Efficiency of the chlorination reaction of the resulting Vilsmeier-Haack reagent. 614.2g POCl 3 Add dropwise to a reaction flask containing 1250ml DMF. Keep the temperature at 0-5°C. Formation of the Vilsmeier-Haack reagent was determined by the formation of an orange color in the flask. The mixture was stirred for 1 hour to complete reagent formation and then the reaction was cooled to -5-0°C. A substrate containing 132 g of sucrose equivalent (sucrose-6-acetate) was added dropwise. The temperature was kept below 0°C during the dropwise addition.

[0042] After the substrate addition was complete, the temperature was allowed to come to room temperature and stirred for 1.0 hour. The temperature was then raised to 65°C and held for 1.5 hours and further heated to 80°C and held for 1.0 hour. The temperature ...

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Abstract

A process is described wherein after formation of first crop of Vilsmeier-Haack reagent, a by-product of the reaction, namely Phosphorus Pentachloride, reacts with N,N-dimethylformamide to form the second crop of Vilsmeier reagent. The PCl5 reacts with N,N-dimethylformamide to obtain the first crop of Vilsmeier reagent as insoluble crystals. The second crop of Vilsmeier reagent is soluble in DMF. This process makes it possible to double the yield of chlorinated substrate, such as sucrose-6-acetate or sucrose-6-benzoate, from the same quantity of Phosphorus Pentachloride.

Description

technical field [0001] The present invention relates to a method and new strategy for synthesizing Vilsmeier-Haack reagent and using said Vilsmeier-Haack reagent to chlorinate sucrose or its derivatives for the production of sucrose, 1'-6'- Chloride of dichloro-1'-6'-dideoxy-β-fructofuranose-4-chloro-4-deoxy-galactopyranoside. Background technique [0002] Prior art strategies for the production of 4,1'6'-sucralose mainly involve the use of the Vilsmeier-Haack reagent (Vilsmeier reagent) to chlorinate sucrose-6-esters, mainly chlorinated sucrose-6-acetate to form 6-acetyl-4,1'6'-sucralose (TGS-6-acetate) or the corresponding chlorinated derivative, which is deacetylated in the reaction mixture itself to form 4,1 '6'-Sucralose (TGS). [0003] As described in U.S. Patent No. 4,380,476 by Mufti et al. (1983), when composed of PCl 5 When producing Vilsmeier-Haack reagent, in PCl 5 Upon reaction with the appropriate tertiary amide, Vilsmeier's reagent was formed as crystals i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H5/00
CPCC07B39/00C07H5/02C01B25/10C07H1/00C07H13/04C07C249/02C07F9/1403C07H13/08C07C251/04C07C251/30
Inventor 雷克莎·拉特纳姆奥萝拉·森迪普莫哈莫德·莫菲朱丁
Owner V B MEDICARE PVT LTD
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