HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diphosgene → HCID 25262942, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | HCID 67543381 | HCID 67543381 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 25262942 | HCID 25262942 | — |
Reaction Steps
115 mg of 2-[3-(2,6-dichlorophenylamino)imidazo[1,2-a]pyrimidin-2-yl]-3,5-dimethoxybenzohydrazide hydrochloride and 26 μl of trichloromethyl chloroformate (diphosgene) are heated under reflux for 2 hours in 5 ml of dioxane. The reaction mixture is evaporated, and water and DCM are added. The aqueous phase is rendered neutral, extracted a number of times with DCM, and the combined organic phases are dried and evaporated. Purification by column chromatography (ethyl acetate/methanol) and washing of the resultant solid by stirring with heptane gives 35 mg (33%) of “A6”; MS-FAB (M+H+)=499.4; Rf (polar method): 1.61 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08278312B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-e02296d405e24fc69606fc22f1e0fb18 |
| Source note | uspto-grants-2012_10 |