HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formic Acid → HCID 178444660, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22141195 | HCID 22141195 | — |
| Solvent | Water | HCID 962 | — |
| Product | Ammonia | HCID 222 | — |
| Product | HCID 178444660 | HCID 178444660 | 40% |
Reaction Steps
A solution of 2-amino-4-(3-hexyl-6-methyl-3-azabicyclo[3.1.0]hex-6-yl)phenylamine (Preparation 48, 112 mg, 0.39 mmol) in formic acid (2.0 ml) was heated under reflux for 1 h. The mixture was cooled, diluted with water (3 ml) and the pH adjusted to 10 with 5N sodium hydroxide. The aqueous layer was extracted with diethyl ether (3×5 ml) and ethyl acetate (2×5 ml). The combined organic layers were dried (MgSO4), filtered and the solvent removed in vacuo. The crude residue was purified by silica columnn chromatography eluting with ethyl acetate then ethyl acetate:methanol:ammonia solution (0.880) (80:20:1) to afford the title compound (46 mg, 40%) as a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313312B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-aa49aa18141a4095b3d8fec2b2fb9b75 |
| Source note | uspto-grants-2001_11 |