HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 59484931, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Triethylamine, 2,2'-dichloro-, hydrochloride | HCID 77142 | — |
| Reactant | HCID 59484949 | HCID 59484949 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 59484931 | HCID 59484931 | — |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
53.3 1.4 g (3.23 mmol) of 2-[3-(5-aminopyrimidin-2-yl)benzyl]-6-(4-methanesulfonylphenyl)-2H-pyridazin-3-one are dissolved in 30 ml of NMP, and 1.59 g (8.72 mmol) of bis(2-chloroethyl)ethylamine hydrochloride and 1.22 g (8.72 mmol) of potassium carbonate are added. The suspension is stirred at 130° C. for 5 days under an argon atmosphere. The reaction mixture is filtered, and the filtrate is stirred into 200 ml of diethyl ether. An oily residue deposits in the process. The residue is purified by means of column chromatography on silica gel. The resultant product is purified by means of preparative HPLC; yield: 41 mg of “A289” trifluoroacetate; HPLC: Rt=2.19 min (method C); LC-MS: 503 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921357B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-8b2b8b6670d94fd0b8a98ec086b37934 |
| Source note | uspto-grants-2014_12 |