Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 11481413 | HCID 11481413 | — |
| Reactant | HCID 18546776 | HCID 18546776 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 11173741 | HCID 11173741 | — |
Reaction Steps
A solution of 1.5 g (0.0068 mol) of 2,4,6-trimethylphenylmalonic acid diamide, 2.16 g (0.0082 mol) of [1,4,5]oxadiazepane dihydrobromide and 2.93 g (0.029 mol) of triethylamine. in 50 ml of xylene is heated for two hours at reflux temperature in a nitrogen atmosphere. The suspension formed is cooled to 22° C., stirred with 1N hydrochloric acid and filtered. The crystalline residue is washed with water and then with diethyl ether and dried in vacuo at 60° C. The desired title compound has a melting point of 248-250° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06552187B1 |
|---|
| Source dataset | uspto-grants-2003_04 |
|---|
| ORD ID | ord-5ecf1bc6c6004da1b6716f3e7ea6c709 |
|---|
| Source note | uspto-grants-2003_04 |
|---|
