HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalyl chloride → HCID 73446015, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 3-Cyano-3-(2-thienyl)acrylic acid potassium salt | HCID 53396629 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 73446015 | HCID 73446015 | 94.8% |
Reaction Steps
To a stirring solution of oxalyl chloride (81.17 mL, 0.93 mol) in CH2Cl2 (350 mL) was added 3-cyano-3-thiophen-2-yl-acrylic acid potassium salt 21 (100 g, 0.45 mol) portion-wise over 20 min. An additional 250 mL of CH2Cl2 were added to assist stirring. The slurry was stirred at room temperature for 30 min and was then filtered. The potassium chloride salts were washed with copious CH2Cl2. Collected organic rinses were combined and solvent removed under vacuum to afford 84.3 g of 22, which was carried on to the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07635695B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-2f8534574f344b848fdc6f33cbfe4136 |
| Source note | uspto-grants-2009_12 |