HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 178503631, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Silicon tetrachloride | HCID 24816 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 68524423 | HCID 68524423 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178503631 | HCID 178503631 | — |
Reaction Steps
Combine 3-(4-tert-butyl-phenyl)-4-cyano-5-methylsulfanyl-thiophene-2-carboxylic acid amide (0.142 mmol) and 1.5 ml CH3CN with NaN3 (0.43 mmol) and SiCl4 (0.142 mmol) in CH2Cl2 and reflux the mixture for 16 hrs. MS shows desired product and starting material. Conc. to dryness and purification by radial chromatography (Si) on a 1000 micron plate eluting with 5% MeOH/0.5% AcOH/CH2Cl2. Concentrate desired fractions to provide the desired title compound: 1H NMR (400 MHz, CDCl3) δ 7.40 (q, 4H, J=22 Hz), 2.73 (s, 3H), and 1.35 (s, 9H), MS found (M+1) 356.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07642361B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-621c37349a744250833d33de31a36a1c |
| Source note | uspto-grants-2010_01 |