HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosgene → HCID 22027861, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 19689608 | HCID 19689608 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22027861 | HCID 22027861 | — |
Reaction Steps
Phosgene in toluene (1.9 ml of a 20% commercial solution, 3.5 mmol) is added within five minutes to a solution of 2-{4-[2-(3-chloro-phenylamino)-pyrimidin-4-yl]-pyridin-2-ylamino}-ethanol (0.88 g, 2.6 mmol) and triethylamine (1.7 ml, 11.7 mmol) in absolute THF (20 ml) at 50° C. After stirring the resulting suspension for one hour at room temperature it is partitioned between ethyl acetate and water. The organic phase is separated, dried over magnesium sulfate, filtered and evaporated under reduced presssure. The residue is purified by silicagel chromatography to give the title compound, m.p. 162–163° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07074787B2 |
| Source dataset | uspto-grants-2006_07 |
| ORD ID | ord-ea1ad38d1a944a9783b596f002b9656b |
| Source note | uspto-grants-2006_07 |