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ChemicalBook CAS DataBase List Triethanolamine borate
283-56-7

Triethanolamine borate synthesis

6synthesis methods
triethanolamine borate synthesis: Adding trimethyl borate into the reaction bottle62.7g (0.6mol), 74.6g (0.5mol) of triethanolamine and 300g of toluene are slowly heated to reflux for 1 hour at room temperature, then distillate is distilled out under normal pressure (65-100°C) while reaction is carried out, sampling is carried out by GC detection, after the reaction is finished, reduced pressure concentration is carried out until no liquid distillation is carried out, acetonitrile is added for recrystallization, filtration and drying are carried out, 68g of white solid is obtained, HPLC (high performance liquid chromatography) is 98.8%, and the yield is 86.6%.
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Yield:283-56-7 87.7%

Reaction Conditions:

in toluene for 1 h;Reflux;Inert atmosphere;Large scale;

Steps:

1.1; 3.1 The first step: the synthesis of triethanolamine borate
Under a nitrogen atmosphere, trimethyl borate.15Kg (49.5mol, 1.1eq), 3.7Kg (45mol, 1eq) of triethanolamine and 18Kg of toluene were charged into a 30L reactor.Slowly raise the temperature to reflux for 1 hour at room temperature.Then, the reaction is distilled to a normal pressure (65 to 100 ° C), and the sample is sampled by GC.After the reaction is completed, the mixture is concentrated under reduced pressure until it is not slipped, and acetonitrile is added for solvent replacement.Recrystallization from 12.3Kg acetonitrile, gradient cooling, filtration,Drying gave 6.2 Kg of white solid, nuclear magnetic purity: 99.0%, yield: 87.7%.

References:

Pulasi Science And Technology (Shanghai) Co., Ltd.;Lu Dianyun;Xiao Haiwang CN109354575, 2019, A Location in patent:Paragraph 0022-0025; 0040-0043

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