HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 5-Dimethylaminoisatoic anhydride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | 2-Amino-5-(dimethylamino)benzoic acid | HCID 12715794 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 5-Dimethylaminoisatoic anhydride | HCID 12715795 | — |
Reaction Steps
To the mixture of 8.9 g of 2-amino-5-dimethylaminobenzoic acid in 60 mL of dioxane, under stirring and external cold water cooling 10 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 7 g of the title product is obtained, m.p.: 258° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071601B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-82d062da84ea46d4b612be3357f7e29d |
| Source note | uspto-grants-2011_12 |