ChemicalBook CAS DataBase List 3,6-DIOXAOCTANEDIOIC ACID

3,6-DIOXAOCTANEDIOIC ACID synthesis

4synthesis methods

Product Name:3,6-DIOXAOCTANEDIOIC ACID
CAS Number:23243-68-7
Molecular formula:C6H10O6
Molecular Weight:178.14

To 15 ml (0.33 mol) of nitric acid was added at 45°C while stirring 1 g of diethylene glycol from the overall amount of 5.9 g (0.06 mol), and the mixture was heated to 65°C. After the end of nitrogen oxides evolution and cooling the mixture to 45-50°C another portion of diethylene glycol was added. Overall time of the reagent addition to the reaction mixture was 1 h. The mixture was kept at 45°C for 40 min and then it was heated at 80°C for 30 min. The solvent was removed in a vacuum at 70°C, the residue was dried by azeotropic distillation with benzene using Dean-Stark trap, then the product was fi ltered off and recrystallized from acetone-benzene mixture. 3,6-Dioxaoctanedioic acid (VIII) was similarly obtained. Yield 7.3 g (89%), colorless crystals. Rf 0.20 (E), mp 76-77°C (mp 75-76°C [13]). IR spectrum, ν, cm-1: 3167 (OH), 2914 (CH), 1733 (C=O acid), 1410, 1229 (C-O), 1121 (C-O). Mass spectrum, m/z (Irel, %): 178.5 [M]+ (76), 200.9 (55), 216.8 (46).

79-11-8
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112-27-6 Synthesis

112-27-6
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23243-68-7
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Yield:23243-68-7 85%

Reaction Conditions:

at 150; for 24 h;

Steps:

1 Example 1 Preparation of ethylenedioxydiacetic acid (L)
Ethylenedioxydiethanol: chloroacetic acid molar ratio of 1: 2
To a 50mL three-neck round bottom flask equipped with a magnetic stirrer, a reflux condenser and a thermometer, add ethylenedioxydiethanol (1mmol) and chloroacetic acid (2mmol). Start the stirring at 150 deg.C. React for 24 hours. After completion of the reaction, the reaction solution was cooled to room temperature, the resulting precipitate was added to 100mL of hot methanol, and stirred to dissolve, filtered, and the filtrate was slowly volatilize give a white solid, yield 85%;

References:

Tianjin Normal University;Wang, Zhongliang CN105669707, 2016, A Location in patent:Paragraph 0018; 0019

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107-21-1 Synthesis