HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 59312283, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 59312360 | HCID 59312360 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59312283 | HCID 59312283 | 66.9% |
Reaction Steps
Zinc dust (943 mg, 14.4 mmol) was added to a mixture of the product from Step B (221 mg, 0.56 mmol) and 0.880 ammonia (20 ml) in tetrahydrofuran (5 ml). This was heated to reflux for 5 h. The reaction mixture was filtered then filtrate was extracted with ethyl acetate (15 ml). The organic phase was dried over magnesium sulphate and concentrated in vacuo. The residue was purified by column chromatography on a silica cartridge, eluting with DCM:MeOH (100:0 to 95:5), to afford the title compound as a pale orange oil in 66.9% yield, 135 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928099B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-4b70d11b7c804cc581b39dfa2745ddef |
| Source note | uspto-grants-2011_04 |