* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
The isosorbide, 1,2-dimethoxyethane, and heteropolyacid were charged into a stainless steel reaction kettle, the autoclave was sealed,The reaction was magnetically stirred at 150 ° C for 5 hours. Wherein the molar ratio of 1,2-dimethoxyethane to isosorbide is 20: 1, heteropoly acidAnd the mass ratio of isosorbide was 0.2: 1. After the reactor was cooled to room temperature, the reaction solution was analyzed by gas chromatography. IsosorbideThe conversion and the yield of its methylated product were calculated in terms of mole percent (molpercent) according to gas chromatography internal standard method.
Reference：
[1] Patent: CN105646514, 2016, A, . Location in patent: Paragraph 0041; 0042; 0043; 0044; 0045; 0046
[2] RSC Advances, 2015, vol. 5, # 31, p. 24139 - 24143
2
[ 150-78-7 ]
[ 652-67-5 ]
[ 162426-86-0 ]
[ 6941-54-4 ]
[ 5306-85-4 ]
Yield
Reaction Conditions
Operation in experiment
17%
at 130℃; for 15 h;
Isosorbide,Methyl etherate and acid catalystAmberlyst-35 was put into a stainless steel reaction kettle,Closed reactor,130 ° C magnetic stirring for 15 hours. among them,The molar ratio of methylating reagent and isosorbide was 50: 1,The mass ratio of catalyst Amberlyst-35 to isosorbide was 0.5: 1. After the reactor was cooled to room temperature,The reaction solution was analyzed by gas chromatography. The conversion of isosorbide and its methylated product yield were calculated by gas chromatography internal standard method,In mole percent.
Reference：
[1] Patent: CN105646514, 2016, A, . Location in patent: Paragraph 0029; 0030; 0031; 0032; 0033; 0034
3
[ 109-87-5 ]
[ 652-67-5 ]
[ 162426-86-0 ]
[ 6941-54-4 ]
[ 5306-85-4 ]
Yield
Reaction Conditions
Operation in experiment
15%
at 130℃; for 15 h;
Isosorbide,Methyl etherate and acid catalystAmberlyst-35 was put into a stainless steel reaction kettle,Closed reactor,130 ° C magnetic stirring for 15 hours. among them,The molar ratio of methylating reagent and isosorbide was 50: 1,The mass ratio of catalyst Amberlyst-35 to isosorbide was 0.5: 1. After the reactor was cooled to room temperature,The reaction solution was analyzed by gas chromatography. The conversion of isosorbide and its methylated product yield were calculated by gas chromatography internal standard method,In mole percent.
Reference：
[1] Patent: CN105646514, 2016, A, . Location in patent: Paragraph 0029; 0030; 0031; 0032; 0033; 0034
4
[ 100-66-3 ]
[ 652-67-5 ]
[ 162426-86-0 ]
[ 6941-54-4 ]
[ 5306-85-4 ]
Yield
Reaction Conditions
Operation in experiment
18%
at 130℃; for 15 h;
Isosorbide,Methyl etherate and acid catalystAmberlyst-35 was put into a stainless steel reaction kettle,Closed reactor,130 ° C magnetic stirring for 15 hours. among them,The molar ratio of methylating reagent and isosorbide was 50: 1,The mass ratio of catalyst Amberlyst-35 to isosorbide was 0.5: 1. After the reactor was cooled to room temperature,The reaction solution was analyzed by gas chromatography. The conversion of isosorbide and its methylated product yield were calculated by gas chromatography internal standard method,In mole percent.
Reference：
[1] Patent: CN105646514, 2016, A, . Location in patent: Paragraph 0029; 0030; 0031; 0032; 0033; 0034
5
[ 109-87-5 ]
[ 111-96-6 ]
[ 652-67-5 ]
[ 162426-86-0 ]
[ 6941-54-4 ]
[ 5306-85-4 ]
Yield
Reaction Conditions
Operation in experiment
18%
at 100℃; for 3 h;
The isosorbide, dimethoxymethane, diethylene glycol dimethyl ether and phosphorus tungsten heteropoly acid into the reaction of stainless steel Kettle, closed reactor, magnetic stirring, at 100 ° C reaction. Among them, the molar ratio of dimethoxymethane and isosorbideIs 30: 1, the molar ratio of diethylene glycol dimethyl ether and isosorbide is 0.5: 1, the mass ratio of phosphotungstic acid to isosorbide is0.5: 1. After the reactor was cooled to room temperature, the reaction solution was analyzed by gas chromatography. Conversion of isosorbide and its methylated product. The yield was calculated according to the gas chromatography internal standard method and expressed in mole percent (ppm).
Reference：
[1] Patent: CN105646514, 2016, A, . Location in patent: Paragraph 0053; 0054; 0055; 0056; 0057; 0058
6
[ 111-96-6 ]
[ 652-67-5 ]
[ 162426-86-0 ]
[ 6941-54-4 ]
[ 5306-85-4 ]
Yield
Reaction Conditions
Operation in experiment
14%
at 200℃; for 2 h;
The isosorbide, diglyme, and acidic catalyst silicotungstic acid were charged into a stainless steel reaction kettle,Sealed reactor, a certain temperature magnetic stirring reaction for 2 hours. Wherein the molar ratio of diethylene glycol dimethyl ether to isosorbide20: 1, and the mass ratio of silicotungsten heteropoly acid to isosorbide was 0.01: 1. The reactor was cooled to room temperature and gas was usedThe reaction solution was analyzed by phase chromatography. The conversion of isosorbide and its methylated product yield were calculated by gas chromatography internal standard method.
Reference：
[1] Patent: CN105646514, 2016, A, . Location in patent: Paragraph 0047; 0048; 0049; 0050; 0051; 0052
7
[ 112-49-2 ]
[ 652-67-5 ]
[ 162426-86-0 ]
[ 6941-54-4 ]
[ 5306-85-4 ]
Reference：
[1] Patent: CN105646514, 2016, A, . Location in patent: Paragraph 0029; 0030; 0031; 0032; 0033; 0034
Isosorbide,Methyl etherate and acid catalystAmberlyst-35 was put into a stainless steel reaction kettle,Closed reactor,130 ° C magnetic stirring for 15 hours. among them,The molar ratio of methylating reagent and isosorbide was 50: 1,The mass ratio of catalyst Amberlyst-35 to isosorbide was 0.5: 1. After the reactor was cooled to room temperature,The reaction solution was analyzed by gas chromatography. The conversion of isosorbide and its methylated product yield were calculated by gas chromatography internal standard method,In mole percent.
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