HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalyl chloride → 4-Chloro-6,7-bis(2-methoxyethoxy)quinazoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 18925053 | HCID 18925053 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4-Chloro-6,7-bis(2-methoxyethoxy)quinazoline | HCID 11289942 | 97.8% |
Reaction Steps
To 6,7-bis(2-methoxy-ethoxy)-quinazolone (500 mg, 1.7 mmol), from Preparation 1, in CHCl3 (10 mL) containing one drop of DMF was added oxalylchloride (490 μL, 5.6 mmol) in several portions over 5 minutes. Once foaming ceased the solution was refluxed 1.5 hours. The solvent was removed in vacuo and the residue was dissolved in 1,2-dichloroethane (20 mL) and washed two times with 80 mL saturated aqueous Na2CO3. The organic phase was dried over Na2SO4, and concentrated in vacuo to afford solid title product (520 mg, 92%; M.P. 108°-109° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE041065E1 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-c803862932644431bd0f0d60a2aea459 |
| Source note | uspto-grants-2009_12 |