HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane hydrochloride → HCID 57686238, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | HCID 86614446 | HCID 86614446 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57686238 | HCID 57686238 | 85.2% |
Reaction Steps
Added 4M HCl/dioxane (2 ml) to a solution of 3-(Formyl-methyl-amino)-1-{2-oxo-2-[4-(4-pyrimidin-2-yl-phenyl)-3,6-dihydro-2H-pyridin-1-yl]-ethyl}-pyrrolidine-3-carboxylic acid [3-(4-fluoro-phenyl)-1trityl-indazol-5-yl]-amide (7T) (89 mg, 0.098 mmol) in MeCl2 (2 ml) at room temperature, then stirred for 2 hours. The solvent was evaporated and the residue extracted with MeCl2 (50 ml), H2O (25 ml) and 3M NaOH (2 ml). The organic layer was separated, dried over MgSO4, filtered and solvent evaporated yielding a solid. Hexanes (2×50 ml) was added and the supernatant decanted. The residual solid was dried yielding 8T as a white solid (55 mg, 84%) LCMS (MH 659) Retention time=2.98 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546404B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-499eb72b627d4edab3412a7573cd2532 |
| Source note | uspto-grants-2013_10 |