HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → HCID 9864542, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Propionyl chloride | HCID 62324 | — |
| Reactant | Phthalazine, 4-[(3,5-dichloro-4-pyridinyl)methyl]-1,2-dihydro-7-methoxy- | HCID 9797215 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9864542 | HCID 9864542 | 86% |
Reaction Steps
A solution of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-1,2-dihydro-phthalazine (1 g, 3.1 mmoles), prepared as described in example 22, in THF (35 ml), under stirring and dry N2 at room temperature, was dropwise added with triethylamine (1.08 ml, 7.76 mmoles), then, at 0° C., with propionyl chloride (0.323 ml, 3.72 mmoles). After 10 minutes the mixture was brought to room temperature and after 3 hours poured into water/ice and THF was evaporated. The mixture was extracted more times with CH2Cl2 and the organic phases were washed with 5% NaOH and water, anhydrified and brought to dryness to give a solid which was crystallised from acetonitrile (50 ml). 1 g of the title compound was obtained (yield: 86%). m.p.: 195-197° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329370B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-6e03a02111b04981beb8abde3534c1f1 |
| Source note | uspto-grants-2001_12 |