HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178498045, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | N-Acetylimidazolidinone | HCID 79350 | — |
| Reactant | Methyl 4-amino-3,5-dichlorobenzoate | HCID 604808 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 178498045 | HCID 178498045 | 75.2% |
Reaction Steps
Methyl-4-amino-3,5-dichlorobenzoate (16.8 g, 31 mmole), 1-acetyl-2-imidazolidone (4.3 g, 33.5 mmole) in phosphoryl chloride (44 ml) were stirred at 50° C. for 3 days. After cooling the phosphoryl chloride was evaporated to give an oily residue. Iced water was added to the residue which was then basified with aqueous sodium hydroxide. The mixture was extracted with methylene chloride which was then washed with water, dried (magnesium sulphate) and evaporated to give a creamy solid. This solid was recrystallised from toluene to give the title compound (7.7 g) mp 188°-189° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04505926 |
| Source dataset | uspto-grants-1985_03 |
| ORD ID | ord-026a6d3952fa4328a8677a98144acf0c |
| Source note | uspto-grants-1985_03 |