HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalyl chloride → Ethyl 5-(3,4-dichlorobenzyl)-1,2,4-oxadiazole-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 3,4-Dichlorophenylacetic acid | HCID 79874 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Ethyl 2-amino-2-(hydroxyimino)acetate | HCID 6785548 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ethyl 5-(3,4-dichlorobenzyl)-1,2,4-oxadiazole-3-carboxylate | HCID 63379228 | 18% |
Reaction Steps
This compound was prepared according to general method 2 with (step I) 2-(3,4-dichlorophenyl)acetic acid (0.775 g; 3.78 mmol) and oxalyl chloride (0.352 mL; 4.16 mmol) in dichloromethane (8 mL) with few drops of DMF and (step II) ethyl 2-amino-2-(hydroxyimino)acetate (0.500 g; 3.78 mmol) and N,N diisopropylethylamine (1.05 mL; 6.06 mmol) in dichloromethane (10 mL) and (step III) pyridine (18 mL). The crude material was purified by flash chromatography on silica (eluent 20 to 100% ethyl acetate in heptane) to yield 0.2004 g (18%) of ethyl 5-(3,4-dichlorobenzyl)-1,2,4-oxadiazole-3-carboxylate as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08618138B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-d56a2804f9b344c6af53a54b14b85c4f |
| Source note | uspto-grants-2013_12 |