1,2-bis(3-(octyloxy)phenyl)ethane-1,2-dione synthesis
- Product Name:1,2-bis(3-(octyloxy)phenyl)ethane-1,2-dione
- CAS Number:1100761-32-7
- Molecular formula:C30H42O4
- Molecular Weight:466.65
Yield:1100761-32-7 55%
Reaction Conditions:
Stage #1: 1-bromo-3-(octyloxy)benzenewith magnesium;lithium bromide;copper(ll) bromide in tetrahydrofuran at 0 - 20; for 0.333333 h;
Stage #2: oxalyl dichloride in tetrahydrofuran at 0; for 0.5 h;
Steps:
1.2 preparation of 1,2 - bis (3-octyloxy-phenyl) benzyl (Compound 2)
LiBr (5.25g, 60.4mmol) was added in THF solution(40ml) of CuBr (4.33g,30.2mmol) and dissolved with stirring at roomtemperature. At ice bath, the temperature was lowered to 0 ° C. The Grignardreagent of m-Bromophenyl octyl ether ((m-Bromophenyl octyl ether 8. 6g, 30.2mmol), Mg(1g, 41.7mmol), THF(30ml)) was added dropwiese. After 20 min ofreaction, oxalyl chloride(1 · 71 g, 13. 5 mmol) was added dropwise under 0 °C,and upon completion of dropping, the reaction was continued for 30min. Into the system saturated NH4Cl solutionwas added to quench the reaction. The system was extracted with ethyl acetate.Theorganic phase was washed with brine and dried over anhydrous MgSO4.Theobtained crude product was concentrated after removal of the organic solvent.Silica gel column chromatography and eluting agent n-hexane / ethyl acetate(200:1,v/v) was used to obtain bis(3-(octyloxy)phenyl) ethane-1,2-dione 3. 46g (Compound 2),with a of yield 55%.
References:
CN102827088,2016,B Location in patent:Paragraph 0037; 0038; 0041; 0042
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