HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 178511692, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Aminocyclohexanol | HCID 81293 | — |
| Reactant | HCID 67370591 | HCID 67370591 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 178511692 | HCID 178511692 | 101% |
Reaction Steps
6.1 g (53 mmol) of 4-amino-cyclohexanol were dissolved in 50 ml of dimethyl acetamide and 4.24 g (106 mmol) of sodium hydride (60%) were added at room temperature. After the reaction mixture was stirred for 30 minutes under argon, a solution of 6.49 g (35.3 mmol) of 6-fluoro-isoquinoline hydrochloride was added and the mixture was stirred at room temperature overnight. For workup, the solvent was removed in vacuo and the residue was dissolved in dichloromethane and washed twice with water. The organic layer was separated, dried with magnesium sulfate and evaporated to yield 8.64 g of the crude product, which was used without further purification. Rt=0.77 min (Method B). Detected mass: 243.1 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796458B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-e915d75041ac41f192e59b19718cd3d6 |
| Source note | uspto-grants-2014_08 |