HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68522041, compound → 3-(4-Iodophenyl)-4-cyano-5-ethyl-thiophene-2-carboxylic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68522041 | HCID 68522041 | — |
| Reactant | HCID 178418750 | HCID 178418750 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(4-Iodophenyl)-4-cyano-5-ethyl-thiophene-2-carboxylic acid ethyl ester | HCID 68522177 | — |
Reaction Steps
Add dropwise diethylzinc (1.0M in hexanes, 16 mmol) to a solution of 3-(4-iodophenyl)-4-cyano-5-methanesulfonyl-thiophene-2-carboxylic acid ethyl ester (2.78 mmol) in 15 mL of anhydrous CH2Cl2 and stir under nitrogen at room temperature for 5 days. Cool to 0° C. and carefully quench with ice followed by 10 mL of saturated NH4Cl. Filter the mixture through Celite and rinse the filter pad with 100 mL of CH2Cl2. Wash the combined organic layers with brine (1×20 mL), dry over Na2SO4, filter, and evaporate. Chromatograph (hexane:ethyl acetate 3:1) over silca gel to provide the title compound: MS (ES+, m/e): 412 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07642361B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-93b78a81ab32493a8351cd11a88d4a44 |
| Source note | uspto-grants-2010_01 |