ChemicalBook CAS DataBase List 3,6-DIACETOXYPHTHALIC ACID ANHYDRIDE

3,6-DIACETOXYPHTHALIC ACID ANHYDRIDE synthesis

4synthesis methods

Product Name:3,6-DIACETOXYPHTHALIC ACID ANHYDRIDE
CAS Number:124511-82-6
Molecular formula:C12H8O7
Molecular Weight:264.19

3786-46-7 Synthesis

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124511-82-6
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Yield:124511-82-6 98.6%

Reaction Conditions:

in 1,2-dichloro-ethane at 85; for 12 h;Solvent;Temperature;

Steps:

3.2 3,6-diacetoxyphthalic anhydride synthesis

1,2-Dichloroethane (1.2 kg),3,6-dihydroxyphthalic acid (0.268 kg, 1.35 mol)And acetic anhydride (0.34 kg, 3.37 mol) were added to the reaction kettle,Heated to 85 degrees, refluxed for 12 hours.The reaction of TLC was complete. Central reaction HPLC showed <2% peak area impurity / product <0.5% of starting material / product. The reaction solution was cooled to room temperature and THF and acetic anhydride were evaporated to dryness. Join PE: EA = 10: 1 mixed beating beating and stirring for 30 minutes. Filter, the filter cake was dried in vacuo to give white crystals 0.352kg (yield: 98.6%).By NMR, it was confirmed that the solid was 3,6-diacetoxyphthalic anhydride.

References:

CN107474007,2017,A Location in patent:Paragraph 0026-0027; 0034-0036; 0043-0045