HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → HCID 178456408, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 1-Bromopropane | HCID 7840 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 178511887 | HCID 178511887 | — |
| Product | HCID 178456408 | HCID 178456408 | — |
Reaction Steps
To N-(2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-2-thiophenecarboximidamide (1.57 g, 6 mmol) in DMF (75 ml) was added potassium carbonate (9 g) and 1-bromopropane (1.48 g, 12 mmol) and a catalytic amount of sodium iodide. The mixture was stirred for 48 h and was then filtered. The solids were dissolved in water (50 ml) and extracted with methylene chloride (3×50 ml). The combined extracts were dried with magnesium sulfate, filtered and concentrated to a solid. The solids were recrystallized from hot isopropanol. The solids were dissolved in ethyl acetate, treated with isopropanol-fumaric acid, and triturated with ether. The hemifumarate salt was collected by filtration (0.86 g, 39%), m.p. 174° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06489322B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-2e5acba7e0854fc5b47942341a2bd57a |
| Source note | uspto-grants-2002_12 |