HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodoethane → 4-(3,5-Dichloro-pyridin-4-ylmethyl)-2-ethyl-7-methoxy-2H-phthalazin-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one | HCID 22482711 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(3,5-Dichloro-pyridin-4-ylmethyl)-2-ethyl-7-methoxy-2H-phthalazin-1-one | HCID 18381676 | 78% |
Reaction Steps
A suspension of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one (0.52 g, 1.55 mmoles), prepared as described in example 38, in DMF (10 ml) was added with NaH (0.057 g, 1.55 mmoles) and, after 1 hour, with ethyl iodide (0.125 ml, 1.55 mmoles). After 1 night the mixture was diluted with water (10 volumes) and extracted twice with ethyl acetate. The organic phase was anhydrified and concentrated to give a solid which was purified by flash chromatography (eluent: ethyl acetate/petrolatum 3:7). There was thus obtained 0.44 g of the title compound (yield: 78%). m.p.: 150.2-151.2° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329370B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-b89c244d43fb40e7b0eb7272043a391e |
| Source note | uspto-grants-2001_12 |