HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178521659, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 9-[8-(2,2,2-Trifluoro-acetyl)-8-aza-bicyclo[3.2.1]oct-3-ylidene]-9H-xanthene-3-carbonitrile | HCID 57725339 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178521659 | HCID 178521659 | — |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
To a solution of Compound 5e (0.232 g, 0.56 mmol) in DMF (5 mL) were added NaN3 (0.11 g, 1.69 mmol) and NH4Cl (0.09 g, 1.68 mmol). The reaction mixture was heated at 120° C. for 14 h, and then cooled to room temperature. An insoluble material was collected by filtration and washed with DMF (5 mL). The filtrate was acidified with 2N HCl (10 mL) and extracted with EtOAc (3×10 mL). The combined organic layers were washed with H2O (10 mL), dried (MgSO4), and concentrated to give the title compound 5f which was used for subsequent reactions without further purification. MS m/z (MH+) 453.9.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07553850B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-3189bd5f9442443ba6607e4c02269a7c |
| Source note | uspto-grants-2009_06 |