ChemicalBook CAS DataBase List HEXAFLUOROGLUTARIC ANHYDRIDE

HEXAFLUOROGLUTARIC ANHYDRIDE synthesis

4synthesis methods

Product Name:HEXAFLUOROGLUTARIC ANHYDRIDE
CAS Number:376-68-1
Molecular formula:C5F6O3
Molecular Weight:222.04

706-79-6
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678-77-3 Synthesis

678-77-3
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376-68-1
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Yield:-

Reaction Conditions:

Stage #1:1,2-dichloro-3,3,4,4,5,5-hexafluorocyclopentene with potassium permanganate;sodium hydroxide; pH=9
Stage #2: with 1H-imidazole;oxalyl dichloride;18-crown-6 ether in dichloromethane at 25; for 2.5 h;

Steps:

4
Add the above mixed salt, 6g imidazole, 10g crown ether (18-crown-6) and 500g dichloromethane together into a 5L three-necked flask with mechanical stirring, constant pressure dropping funnel and thermometer catheter.Under stirring conditions, 600 g of oxalyl chloride was dropped into the flask through a constant pressure dropping funnel, and the internal temperature was controlled at about 25°C. The exhaust gas is absorbed by lye.After the addition was completed in 2h, stirring was continued for 0.5h to end the reaction. A dry ice alcohol cold trap was used to collect the distilled products under reduced pressure (80, ≤20mmHg), and the corresponding contents of hexafluoroglutarate and hexafluoroglutaric anhydride were 64.3% and 34.9% by GC analysis.

References:

Zhong Lan Chenguang Chemical Design Yuan Co., Ltd.;Luo Kai;Luo Shengqiao;Chen Binbin;Dou Ruoan;Hu Jun;Gan Libing;Lai Bihong CN111333501, 2020, A Location in patent:Paragraph 0037-0038