Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzoic Acid | HCID 243 | — |
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 54064120 | HCID 54064120 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 15295811 | HCID 15295811 | — |
Reaction Steps
145 mg of benzoic acid and 192 mg of carbonyldiimidazole are stirred in 1 ml of tetrahydrofuran for 2 hours at 50° C. To this is added a solution of 163 mg of 4'-[(2-n-propyl-4-methyl-6-(1-methylbenzimidazol-2-yl)-benzimidazol-1-yl)-methyl]-2-sulphamoyl-biphenyl, 0.133 ml of 1,8-diazabicyclo-[5.4.0]undec-7-ene and 1 ml of tetrahydrofuran and the mixture is maintained at 55° C. for 2.5 hours. Then 50 ml of ethyl acetate and 20 ml of 5% citric acid are added. The organic phase is dried with sodium sulphate and evaporated down. The residue obtained is chromatographed over silica gel with dichloromethane/ethanol (95:5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05565469 |
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| Source dataset | uspto-grants-1996_10 |
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| ORD ID | ord-8d19d475967b4e5a984f4a044dec614a |
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| Source note | uspto-grants-1996_10 |
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