Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| Reactant | 4-Chloro-1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxyphthalazine | HCID 18629210 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dimethyl sulfoxide methanol | HCID 22036561 | — |
| Product | HCID 54227958 | HCID 54227958 | 726.4% |
Reaction Steps
A suspension of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (9.7 g, 27 mmoles), prepared as described in example 45, in DMSO/CH3OH (80/40 ml) was added with K2CO3 (7.4 g, 54 mmoles), palladium acetate (0.31 g, 1.4 mmoles) and 1,3-bis(diphenylphosphine)propane (0.75 g, 1.82 mmoles). The mixture was placed in autoclave under CO atmosphere (8 bar) and heated at 50° C. After 4 hours the mixture was poured into water (10 volumes) and extracted four times with ethyl acetate. The organic phase was washed with aqueous NaCl and discoloured with charcoal, filtered and dried to give a solid which was flash chromatographed (eluent: petrolatum/ethyl acetate 1:1) to give 5 g of the title compound (yield: 49%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06492360B1 |
|---|
| Source dataset | uspto-grants-2002_12 |
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| ORD ID | ord-0f2446b2aab542efa6806e35e01a7423 |
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| Source note | uspto-grants-2002_12 |
|---|
