HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine hydrochloride → HCID 49764059, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine hydrochloride | HCID 11130 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 49764057 | HCID 49764057 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 49764059 | HCID 49764059 | — |
Reaction Steps
A solution of N-({1-[4-(4-cyanomethyl-phenyl)-cyclohexyl]-azetidin-3-ylcarbamoyl}-methyl)-3-trifluoromethyl-benzamide (as prepared in Example 21, 250 mg, 0.50 mmol), sodium azide (Aldrich, 160 mg, 2.50 mmol), and Et3N HCl salt (350 mg, 2.50 mmol) in dioxane (5 mL) was heated in a sealed tube to 120° C. overnight. The solvent was removed in vacuo and the residue was purified on a silica gel column using a CombiFlash® system using ethyl acetate and 7N NH3 in MeOH as eluent (from pure ethyl acetate to 5% 7N NH3 in MeOH in ethyl acetate) to afford the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08513229B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-66daab7cebf6435480775fd81962ea86 |
| Source note | uspto-grants-2013_08 |