HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen iodide → HCID 18465001, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen iodide | HCID 24841 | — |
| Reactant | HCID 70148112 | HCID 70148112 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 18465001 | HCID 18465001 | 95.4% |
Reaction Steps
Treat a stirred solution of 4-(1-vinyl-1H-benzoimidazol-2-yl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester (0.97 g, 2.8 mmol) and methanol (20 mL) at 0° C. with 57% hydroiodic acid (467 microliters, 6.21 mmol) solution. Stir at room temperatue for two hours, add 57% hydroiodic acid (934 microliters) and reflux for 30 minutes. Cool to room temperature, concentrate in vacuo to approximately 5 mL final volume, and add ether (total of 200 mL) to afford a tacky solid. Stir the suspension overnight, collect the solid by filtration under nitrogen and dry in vacuo for two hours. Dry in vacuo (0.2 Torr) at room temperature overnight to afford 1.33 g of 2-[1,4]diazepan-1-yl-1-vinyl-1H-benzoimidazole dihydroiodide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06423704B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-ed82fa423a624a27af3b663f73259f84 |
| Source note | uspto-grants-2002_07 |