HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethyl orthoacetate → HCID 21936603, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethyl orthoacetate | HCID 15050 | — |
| Reactant | Tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy)ethylcarbamate | HCID 12106200 | — |
| Reactant | Pyridinium hydrochloride | HCID 21584435 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 21936603 | HCID 21936603 | 83.5% |
Reaction Steps
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (12.05 g, 34.8 mmol) in 200 mL of 1,2-dichloroethane was treated with trimethyl orthoacetate (5.50 mL, 43.2 mmol) and the reaction mixture was heated to reflux. A 100 mg portion of pyridinium hydrochloride was then added and refluxing was continued for 4 h. The reaction was then cooled and washed with water and brine. The organic portion was dried over Na2SO4 and concentrated to give an orange foam. The foam was triturated with ether and filtered to yield 10.76 g of tert-butyl 2-[2-(2-methyl-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate as a tan solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115622B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-874d3d3fb1384cb2891903091ef9315f |
| Source note | uspto-grants-2006_10 |