HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 18464457, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Emedastine EP Impurity E | HCID 9984168 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 18464457 | HCID 18464457 | — |
Reaction Steps
Combine 4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (5.10 g, 1.8 mmol) and 48% hydrobromic acid (25 mL). Heat to reflux. After 18 hours, dilute with water and adjust the pH to 12 using aqueous 5 M sodium hydroxide solution. Extract three times with dichloromethane. Dry the combined organic layers over Na2SO4, filter, and evaporate in vacuo to give a residue. Combine the residue and methanol (50 mL). Add a solution of hydrochloric acid (5.0 mL, 4 M, 20 mmol) in dioxane. Evaporate in vacuo to give a residue. Triturate the residue with diethyl ether to give a solid. Collect the solid by filtration and dry to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194406B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-dbd9fbd33d7a4e26b8cc4b744a271c9a |
| Source note | uspto-grants-2001_02 |