Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cetyl Alcohol | HCID 2682 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 12780501 | HCID 12780501 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19899498 | HCID 19899498 | 95.3% |
Reaction Steps
4'-Methanesulfonyl-2,2':6',2"-terpyridine (4.67 g, 0.015 mol) and hexadecyl alcohol (2.42 g, 0.010 mol) were added to N,N-dimethylformamide (0.1 liter). At 15°C., sodium hydride (60% content, oil dispersion, 0.8 g) was added thereto over a period of about 10 minutes. The entire solution was stirred for 30 minutes and then the reaction mixture was reacted under reflux for 4 hours. After cooling to room temperature, the reaction mixture was poured into an aqueous 4 M sodium chloride solution (0.3 liter). The crystal that precipitated was taken out by filtration under suction and then washed with water and hexane. The crystal was again dissolved in chloroform and washed with 1 M hydrochloric acid and water. The organic layer was dried over anhydrous sodium sulfate and then concentrated. The resulting crystal was recrystallized from hexane to obtain 4.36 g of the above-entitled product (T-6). Yield: 92%. m.p. 97.5° to 99.0° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04960895 |
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| Source dataset | uspto-grants-1990_10 |
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| ORD ID | ord-a3682bf28dd84cabb77cd955f076c2cc |
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| Source note | uspto-grants-1990_10 |
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