Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 22272701 | HCID 22272701 | — |
| Reactant | HCID 69731041 | HCID 69731041 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 22272628 | HCID 22272628 | 88.5% |
Reaction Steps
To a solution of this phenyl carbamate (1.46 g, 4.19 mmol) in toluene (20 ml) were added triethylamine (509 mg, 5.03 mmol) and 2-[4-(2-heptylaminoethyl)piperazin-1-yl]ethanol (1.14 g, 4.20 mmol) obtained in Example 16 and the mixture was stirred at 80° C. for 2 hours. The reaction solution was diluted with water and extracted with chloroform. The organic layer was washed with water and a saturated sodium chloride solution successively, dried over anhydrous sodium sulfate and concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (silica gel 100 g, developing solvent; chloroform:methanol=40:1 20:1) to provide 1.95 g (yield 88%) of N′-[2,4-bis(ethylthio)-6-methyl-3-pyridyl]-N-heptyl-N-[2-[4-(2-hydroxyethyl)piperazin-1-yl]ethyl]urea as pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06969711B2 |
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| Source dataset | uspto-grants-2005_11 |
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| ORD ID | ord-4ec9b1dfb8684073b0838358267fca04 |
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| Source note | uspto-grants-2005_11 |
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