Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,6-Dimethoxybenzoic Acid | HCID 15109 | — |
| Reactant | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Reactant | HCID 19769907 | HCID 19769907 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 19769912 | HCID 19769912 | 12.9% |
Reaction Steps
To 1 g (6.41 mmol) of 2,6-dimethoxybenzoic acid, were added 10 ml of toluene, 1.05 ml (6.79 mmol) of triethylamine and 1.41 ml (6.54 mmol) of diphenylphosphoryl azide and stirred at 100° C. for one hour. The reaction solution was cooled to room temperature, then added with a 5 ml of toluene solution of 1.40 g (6.41 mmol) of 2-(3,4-methylenedioxyphenyl)-hexylamine and stirred overnight at room temperature. The thus treated reaction solution was purified by silica gel column chromatography (developed with a 2/1 mixture of hexane and ethyl acetate) and then recrystallized from the hexane/ethyl acetate mixed solvent to obtain 330 mg of 1-(2-(3,4-methylenedioxyphenyl)hexyl)-3-(2,6-dimethyoxyphenyl)urea (yield: 12.9%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05202351 |
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| Source dataset | uspto-grants-1993_04 |
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| ORD ID | ord-b2cf3e30e73044a1b8a85389824bc4cc |
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| Source note | uspto-grants-1993_04 |
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