HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 58487596, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 3-Benzyl-3-azabicyclo[3.1.0]hexane-1-carboxylic acid | HCID 15713431 | — |
| Product | HCID 58487596 | HCID 58487596 | — |
Reaction Steps
To a suspension of 3-benzyl-3-azabicyclo[3.1.0]hexane-1-carboxylic acid (8.5 gm, 0.0390 mole), (prepared as described in EP 0413455A2) in ethyl alcohol (250 ml) was added conc. H2SO4 (10 ml). The resulting pale yellow solution was heated at reflux for 2 hours, cooled to 0° C. and neutralized with aqueous ammonia. The neutralized solution was concentrated and was dissolved in dichloromethane. The organic layer was washed with saturated NaHCO3, water and brine. The organic layer was dried over anhydrous Na2SO4 and was concentrated to give the crude product which was further purified by column chromatography (100-200 mesh, silicagel), eluting the compound with 5% ethyl acetate in hexane to give the pure product as yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592359B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-f2bebf234f20439ba3a03b8a4cf3ad56 |
| Source note | uspto-grants-2009_09 |