HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → 1-(3,5-Dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine 3-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 9927063 | HCID 9927063 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(3,5-Dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine 3-oxide | HCID 18381665 | 31% |
Reaction Steps
A solution of 1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (1 g, 3.13 mmoles), prepared as described in example 5, in dry CH2Cl2 (15 ml), under stirring and N2 at room temperature, was added with m-chloroperbenzoic acid (0.81 g, 4.7 mmoles). After 1 hour the mixture was washed with 10% NaOH and water, anhydrified and brought to dryness. The residue was flash chromatographed (eluent: ethyl acetate 100%, then ethyl acetate/CH3OH 8:2) to give a solid which was crystallised from acetic acid/ethyl acetate to give 0.32 g of the title compound (yield: 31%). m.p.>230° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329370B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-7fde72c0f0cf427cb7dbe40e8cdd80ca |
| Source note | uspto-grants-2001_12 |