HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → 5-(6-Aminopyridin-3-yl)piperidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | (6-Fluoropyridin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)piperidin-2-one | HCID 131734604 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 5-(6-Aminopyridin-3-yl)piperidin-2-one | HCID 118045436 | — |
Reaction Steps
To -(6-fluoropyridin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)piperidin-2-one (290 mg, 0.894 mmol) in a steel bomb, ammonium hydroxide (34.8 μl, 0.894 mmol) solution was added (40% head volume remained). The steel bomb reactor was heated at 150° C. for 44 h (250 psi on pressure gauge). LCMS—0.23 min, MH+192.1 (without SEM); 0.66 min, MH+322.1 (with SEM). After diluted with MeOH and toluene, volatile materials were completely removed in vacuo. 5-(6-aminopyridin-3-yl)piperidin-2-one was used for the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242996B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-ab11cc6df8af47e69d2cc0cfc725a106 |
| Source note | uspto-grants-2016_01 |