HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86607777, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | 2-AMino-5-(4-Methyl-1-piperazinyl)benzoic Acid | HCID 50989007 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86607777 | HCID 86607777 | — |
Reaction Steps
To the mixture of 5.3 g of 2-amino-5-(4-methylpiperazino)benzoic acid in 30 mL of dioxane, under stirring and external cold water cooling 6 mL of diphosgene is added dropwise. The mixture is heated under reflux conditions for 4 hours. From the cold reaction mixture the solid material is filtered off, washed with 50 mL of ether. The product is stirred for 5 minutes in the mixture of 50 mL of methanol and 5 mL of triethylamine, filtered off, washed with 30 mL of methanol. After drying 5.4 g of the title product is obtained, m.p.: 285° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07547696B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-186b3899e251477585ac72f4473f4df1 |
| Source note | uspto-grants-2009_06 |