HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86646771, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Cyanamide | HCID 9864 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 57467435 | HCID 57467435 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86646771 | HCID 86646771 | — |
Reaction Steps
To a solution of sodium ethoxide in ethanol, freshly prepared from sodium (0.02 mol) and ethanol (50 mL), was added 2-methyl-2-phenoxypropanenitrile from Step D (0.05 mol). The mixture was stirred overnight at room temperature, and then acetic acid (0.07 mol) was added, followed by addition of NH2CN (0.05 mol). The mixture was stirred for 3 hours and the solvent was removed. The residue was purified by column chromatography on silica gel (mobile phase: petroleum ether/ethyl acetate=4:1˜1:1) to give the titled compound. 1H NMR (400 MHz, CDCl3) δ ppm 7.27 (t, J=8.0 Hz 2H), 7.05 (t, J=7.2 Hz 1H), 6.88˜6.90 (m, 2H), 4.38 (q, J=7.2 Hz, 2H), 1.61 (s, 6H), 1.39 (t, J=7.2 Hz, 3H); LCMS (ESI+) m/z 233 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08507493B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-bc503395b0dd4edc9d94b1d7adf9916d |
| Source note | uspto-grants-2013_08 |