Synthesis of sucrose-6-acetate

A synthesis method and acetate technology, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of complex process and high production cost, and achieve simple process, low production cost and high product purity. Effect

Inactive Publication Date: 2004-11-17
广东广业清怡食品科技股份有限公司
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  • Abstract
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Problems solved by technology

[0007] The synthetic method of sucrose-6-acetate mainly contains two kinds: ethyl acetate method (as U.S. Pat. The synthe

Method used

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  • Synthesis of sucrose-6-acetate
  • Synthesis of sucrose-6-acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Preparation of supported cerium sulfate-silica gel catalyst

[0015] Add 6.2g Ce(SO 4 ) 2 4H 2 O, add 20ml of water to dissolve, then add 4.8g of 230-400 mesh silica gel, heat to 110°C on a rotary evaporator and dry under vacuum (200Pa) for 3 hours to obtain about 9.5 grams of cerium sulfate-silica gel (1:1) catalyst.

Embodiment 2

[0017] In a 1000ml three-necked flask, add 50g of sucrose, 250ml of N,N-dimethylformamide (DMF), 2g of anhydrous cerium sulfate and 50ml of ethyl acetate, heat to 80°C and stir for 4 hours, then cool to 10°C , filter and recover cerium sulfate, first distill off the unreacted ethyl acetate at room temperature, and then distill all the DMF under reduced pressure. Obtain 55g of syrup, detect by HPLC, the content of sucrose-6-acetate is 79.3%.

Embodiment 3

[0019] In a 1000ml three-necked flask, add 50g of sucrose, 250ml of N,N-dimethylformamide (DMF), 5g of cerium sulfate-silica gel (1:1), 100ml of ethyl acetate, heat to 80°C and stir for 4 hours , cooled to 5°C, and the catalyst was recovered by filtration. First, the unreacted ethyl acetate was evaporated at room temperature, and then all the DMF was evaporated under reduced pressure to obtain 56 g of syrup. The content of sucrose-6-acetate was 85.7% by HPLC detection.

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Abstract

The present invention discloses the synthesis of sucrose-6-acetate. Sucrose material is mixed with N, N-dimethyl formamide solution, made to produce ester exchange reaction with ethyl acetate under the action of solid sulfate catalyst, which may be adsorbed on polymer carrier, to produce sucrose-6-acetate. Sucrose-6-acetate is the key intermediate for synthesizing trichlorosucrose as sweetening agent. The present invention has the advantages of simple technological process, high product purity, low production cost, etc. and is suitable for industrial production.

Description

Technical field [0001] The invention relates to a method for synthesizing sucrose-6-acetate, a key intermediate for synthesizing sweetener sucralose. Background technique [0002] Sucralose, chemical name 4,1',6'-trichloro-4,1',6'-trideoxygalactose, its structural formula is: [0003] [0004] Sucralose is 600 times sweeter than sucrose and has been approved as a food sweetener by more than 20 countries. [0005] The preparation methods of sucralose generally fall into two categories: single group protection method and whole group protection method. The whole group protection method (as recorded in US Pat. To make other hydroxyl groups react while the 6-position hydroxyl group remains unchanged, group protection of the 6-position hydroxyl group is required, which is the starting point for the consideration of single-group protection. Therefore, the core of the single-group protection method is the preparation of sucrose-6-acetate. The structural formula of sucrose-6-a...

Claims

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Application Information

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IPC IPC(8): C07H13/06
Inventor 王三永李春荣
Owner 广东广业清怡食品科技股份有限公司
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