HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 18332464, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 4-Chloro-1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxyphthalazine | HCID 18629210 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18332464 | HCID 18332464 | 1,179.1% |
Reaction Steps
A solution under N2 of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (1.3 g, 3.7 mmoles), prepared as described in example 45, in dry DMF (50 ml) was added with K2CO3 (1.28 g, 9.25 mmoles), palladium acetate (0.017 g, 0.074 mmoles), CuI (0.028 g, 0.15 mmoles), and triphenylphosphine (0.58 g, 0.22 mmoles). After 30 minutes under stirring 4-prop-2-ynyl-morpholine (1.16 g, 9.25 mmoles) was added and the mixture was stirred overnight, poured into water (10 volumes) and extracted twice with ethyl acetate. After decolouring with charcoal, filtering over celite, concentrating and triturating in ethyl ether, 1.15 g of the title compound were obtained (yield: 70%). m.p.: 171.7-172.7° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329370B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-9b4171c35cc046debf3c40e24790db32 |
| Source note | uspto-grants-2001_12 |