HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → 1-Chloro-4-ethyl-6-methoxy-phthalazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 4-ethyl-6-methoxy-2H-phthalazin-1-one | HCID 18381611 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-Chloro-4-ethyl-6-methoxy-phthalazine | HCID 18381645 | 89% |
Reaction Steps
A suspension of 4-ethyl-6-methoxy-2H-phthalazin-1-one (1.3 g, 6.76 mmoles), prepared as described in example 9, in dry acetonitrile (20 ml), under stirring and dry N2 at room temperature, was added with phosphorous oxychloride (2.07 g, 13.52 mmoles). The mixture was refluxed and after 2 hours cooled, brought to small volume, taken up in water, added with Na2CO3 in excess and extracted three times with CH2Cl2. The organic phases were anhydrified and brought to dryness to give 1.34 g of the title compound (yield: 89%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06492360B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-b4c04b0586874ccbaace943eea67512b |
| Source note | uspto-grants-2002_12 |