Preparation method of electronic grade octyl gallate
A technology of octyl gallate and gallic acid is applied in the preparation of carboxylate, the preparation of organic compounds, the preparation of ester group and hydroxyl reaction, etc., can solve the problems of high catalysis cost of metal palladium, easy to have heavy metal residues and the like, and achieve low cost Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0024] The first step: the synthesis of gallate:
[0025] Synthesis of methyl gallate:
[0026]
[0027] Put 400g of methanol and 85g (0.5mol) of gallic acid into the reaction bottle, slowly add 71.4g (0.6mol) of thionyl chloride dropwise at room temperature, keep the temperature at 35-40°C, after the dropwise addition, raise the temperature to reflux for 1 hour , Sampling detection (HPLC) whether the reaction is complete, the ratio of product to raw material is 50:1 to determine the end of the reaction, after the reaction is completed, concentrate to a smooth liquid, drop 300g of water into the slurry at room temperature for 1 hour, filter, and dry. Obtained 86.2g product, HPLC: 98.8%, yield: 93.6%. 1H NMR (400MHz, DMSO): 9.16 (m, 3H), 6.94 (s, 2H), 1.26 (m, 3H).
[0028] Synthesis of ethyl gallate:
[0029]
[0030] Put 400g of ethanol and 85g (0.5mol) of gallic acid into the reaction bottle, slowly drop into 71.4g of thionyl chloride at room temperature, keep the t...
Embodiment 2
[0041] The second step: the synthesis of octyl gallate.
[0042]
[0043]27.4g (0.21mol) of n-octanol, 36.8g (0.2mol) of methyl gallate, 2g (0.004mol) of three (pentafluorophenyl) boranes and 350g of toluene are dropped into the reaction bottle, and as the temperature rises, the system becomes For clarification, slowly increase the value and reflux reaction for 3 to 4 hours, sample HPLC to detect that the raw material is <0.5%, and carry out post-treatment. Add 6.7g of mercapto silica gel to the material being refluxed to capture heavy metals, heat filter, concentrate the filtrate and recover the solvent, then drop into 150g of water for beating at room temperature, filter, and dry to obtain 53g of octyl gallate of electronic grade, HPLC: 99.1% , Yield: 93.9%. 1HNMR (400MHz, DMSO): 9.16(s, 3H), 6.94(s, 2H), 4.15(t, 2H), 1.64(dd, 2H), 1.45-1.21(m, 10H), 0.86(t, 3H) .
[0044]
[0045] In reaction flask, drop into n-octanol 27.4g (0.21mol), ethyl gallate 39.6g (0.2mol),...
Embodiment 3
[0054] The first step: the synthesis of methyl gallate:
[0055]
[0056] Put 31Kg of methanol and 7.65Kg (45mol, 1eq) of gallic acid into the 50L reactor, slowly drop 5.85Kg (1.1eq) of thionyl chloride into the 50L reaction kettle, and keep the temperature at 35-40°C. After the addition, the temperature was raised to Reflux for 1 hour, take a sample to check (HPLC) whether the reaction is complete, the ratio of product to raw material is 50:1 to determine the end point of the reaction, after the reaction is completed, concentrate to a smooth liquid, drop into 28Kg water for beating at room temperature for 1 hour, filter, and dry. Obtain 8Kg product, HPLC: 98.6%, yield: 96.6%.
[0057] The second step: the synthesis of octyl gallate.
[0058]
[0059] 5.95Kg (0.21mol, 1.05eq) of n-octanol, 8Kg (43.5mol, 1eq) of methyl gallate, 0.22Kg (0.01eq) of tris(pentafluorophenyl) borane and chlorobenzene were put into the 50L reactor. 32kg, as the temperature rises, the system be...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More