N-METHYLTETRAFLUOROPHTHALIMIDE synthesis
- Product Name:N-METHYLTETRAFLUOROPHTHALIMIDE
- CAS Number:33795-85-6
- Molecular formula:C9H3F4NO2
- Molecular Weight:233.12
14737-80-5
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$100.00/250mg
33795-85-6
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$65.00/5g
Yield: 96.6%
Reaction Conditions:
Stage #1:N-methyl-tetrachlorophthalimide with potassium fluoride in dimethyl sulfoxide at 160; for 6 h;
Stage #2: with potassium fluoride;aniline in dimethyl sulfoxide at 160; for 6 h;Solvent;Temperature;
Steps:
25 Example 1-1
General procedure: Pre-fluorination: in 60 ml of DMSO,Will be dryN-methyl tetrachlorophthalimide5 g (0.0167 mol) and 3.89 g (0.067 mol) of potassium fluoride as a fluorinating agent were mixed and reacted at 140 ° C for 4 hours.The reaction was light yellow reaction solution I, cooled to room temperature and filtered,A white cake I (whose main component is potassium chloride) and a filtrate I (a light yellow partially fluorinated solution) was obtained.Perfluorination: 3.89 g (0.067 mol) of potassium fluoride was added to the filtrate I obtained by the pre-fluorination,The reaction was carried out at 140 ° C for 4 hours to obtain a reaction solution II (light yellow perfluorinated solution)After cooling to room temperature,A white cake II (containing about 68-70% potassium fluoride,The rest is potassium chloride) and filtrate II (light yellow perfluorinated solution).The filtrate II was distilled off under reduced pressure (10 mmHg) to give the crude N-methyltetrafluorophthalamide (pale yellow powder).Pre-fluorination consumption KF2.79g, perfluorinated consumption KF0.87g,The feed conversion was 100%, partial fluoride was 21.5%The crude product was recrystallized from THF / H2O (2: 1, v: v)The yield of N-methyltetrafluoro-phthalimide was 78.5%.
References:
Zhejiang University;Chen Xinzhi;Gao Rui;Qian Chao CN106565590, 2017, A Location in patent:Paragraph 0036; 0037; 0038; 0039; 0040; 0041-0047
14737-80-5
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$100.00/250mg
2751-90-8
446 suppliers
$7.00/25g
33795-85-6
62 suppliers
$65.00/5g
117-08-8
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33795-85-6
62 suppliers
$65.00/5g