Technology Process of 4,4'-{(1E,3E,5E,7Z,9E,11Z,13E,15E,17E)-7-(4-bromophenyl)-4,15-dimethyl-12-p-tolyloctadeca-1,3,5,7,9,11,13,15,17-nonaene-1,18-diyl}bis(4,1-phenylene)bis(methylsulfane)
There total 7 articles about 4,4'-{(1E,3E,5E,7Z,9E,11Z,13E,15E,17E)-7-(4-bromophenyl)-4,15-dimethyl-12-p-tolyloctadeca-1,3,5,7,9,11,13,15,17-nonaene-1,18-diyl}bis(4,1-phenylene)bis(methylsulfane) which
guide to synthetic route it.
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synthetic route:
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1450630-16-6
4,4'-{(1E,3E,5E,7Z,9E,11Z,13E,15E,17E)-7-(4-bromophenyl)-4,15-dimethyl-12-p-tolyloctadeca-1,3,5,7,9,11,13,15,17-nonaene-1,18-diyl}bis(4,1-phenylene)bis(methylsulfane)
- Guidance literature:
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With
potassium methanolate;
In
cyclohexane; benzene;
at 80 - 90 ℃;
for 12h;
Inert atmosphere;
DOI:10.1002/chem.201300984
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1450630-16-6
4,4'-{(1E,3E,5E,7Z,9E,11Z,13E,15E,17E)-7-(4-bromophenyl)-4,15-dimethyl-12-p-tolyloctadeca-1,3,5,7,9,11,13,15,17-nonaene-1,18-diyl}bis(4,1-phenylene)bis(methylsulfane)
- Guidance literature:
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Multi-step reaction with 2 steps
1: phosphorus pentoxide / 18 h / 20 °C / Inert atmosphere
2: potassium methanolate / cyclohexane; benzene / 12 h / 80 - 90 °C / Inert atmosphere
With
phosphorus pentoxide; potassium methanolate;
In
cyclohexane; benzene;
DOI:10.1002/chem.201300984
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-
1450630-16-6
4,4'-{(1E,3E,5E,7Z,9E,11Z,13E,15E,17E)-7-(4-bromophenyl)-4,15-dimethyl-12-p-tolyloctadeca-1,3,5,7,9,11,13,15,17-nonaene-1,18-diyl}bis(4,1-phenylene)bis(methylsulfane)
- Guidance literature:
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Multi-step reaction with 6 steps
1.1: potassium tert-butylate / N,N-dimethyl-formamide / 0.5 h / -20 °C / Inert atmosphere
1.2: 1.5 h / -20 °C / Inert atmosphere
2.1: lithium aluminium tetrahydride / tetrahydrofuran / 0.5 h / 0 °C / Inert atmosphere
3.1: oxalyl dichloride / dichloromethane; dimethyl sulfoxide / 1 h / -78 °C / Inert atmosphere
3.2: 2 h / -78 °C / Inert atmosphere
4.1: n-butyllithium / tetrahydrofuran; hexane / 0.5 h / -78 °C / Inert atmosphere
4.2: 2.08 h / -78 °C / Inert atmosphere
5.1: phosphorus pentoxide / 18 h / 20 °C / Inert atmosphere
6.1: potassium methanolate / cyclohexane; benzene / 12 h / 80 - 90 °C / Inert atmosphere
With
lithium aluminium tetrahydride; n-butyllithium; oxalyl dichloride; phosphorus pentoxide; potassium methanolate; potassium tert-butylate;
In
tetrahydrofuran; hexane; dichloromethane; cyclohexane; dimethyl sulfoxide; N,N-dimethyl-formamide; benzene;
3.1: |Swern Oxidation / 3.2: |Swern Oxidation;
DOI:10.1002/chem.201300984