HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxide (P4O10) → 6,7-Dichloro-3,4-dihydro-2H-isoquinolin-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Reactant | HCID 66802053 | HCID 66802053 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | 6,7-Dichloro-3,4-dihydro-2H-isoquinolin-1-one | HCID 14177101 | 20.3% |
Reaction Steps
Using an analogous procedure and workup as described for the preparation of intermediate I-1d above, ethyl 3,4-dichlorophenethylcarbamate (I-55c: 6 g, 22.989 mmol) in POCl3 (60 mL) was reacted with P2O5 (6.52 g, 45.977 mmol) at 120° C. for 1 hour to afford the crude product. Purification by column chromatography on silica gel (30% ethylacetate in hexane) afforded 1.01 g of the product. LCMS: 53.61%, m/z=216.0 (M+1)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946260B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-e46051135ec24ace956c5cd3c6f29d58 |
| Source note | uspto-grants-2015_02 |