HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bis(2-amino-1H-imidazole) sulphate → HCID 178522543, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bis(2-amino-1H-imidazole) sulphate | HCID 135136 | — |
| Reactant | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| Reactant | HCID 178524177 | HCID 178524177 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Diisopropylethylamine | HCID 81531 | — |
| Product | HCID 178522543 | HCID 178522543 | 5.6% |
Reaction Steps
0.15 g (0.45 mmol) of 2-[(isoquinoline-3-carbonyl)-amino]-1H-benzoimidazole-5-carboxylic acid was reacted with 0.26 g (0.68 mmol) of HBTU and 0.06 g (0.45 mmol) of 2-aminoimidazole sulfate in 3.0 mL of DMF and 1.0 mL of DIEA as described in general procedure A. After cooling to room temperature, the reaction mixture was diluted with water, the solid was collected by filtration, dissolved with MeOH and evaporated onto silica gel, and isolated by flash column chromatography (500 mL DCM/20 mL NH3/MeOH) to yield ˜10 mg of the desired isoquinoline-3-carboxylic acid [5-(1H-imidazol-2-ylcarbamoyl)-1H-benzoimidazol-2-yl]-amide. LCMS: 398.0 (M+1)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598353B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-82f185965cf7429d88d3e99df7d9b1ea |
| Source note | uspto-grants-2013_12 |