HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 54002860, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Acetic acid, 2-hydrazinyl-, ethyl ester, hydrochloride (1:1) | HCID 11593468 | — |
| Reactant | 2-Cyano-3-methylthio-3-(4-tolyl)acrylamide | HCID 54242237 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54002860 | HCID 54002860 | 27.5% |
Reaction Steps
The title compound was prepared from 2-cyano-3-methylthio-3-(4-tolyl)acrylamide (425 mg, 1.83 mmol), ethyl hydrazinoacetate hydrochloride (311 mg, 2.01 mmol) and sodium hydroxide (80 mg, 2.01 mmol) following the procedure used for the compound of Example 12. The crude product was subjected to column chromatography (SiO2, 10% methanol in CH2Cl2) and was recrystallised from ethyl acetate to give the title compound as white crystals (152 mg) m.p. 179°. δH (CDCl3) 7.43 (2H, d, J 8.1 Hz), 7.26 (2H, d, J 8.1 Hz), 5.56 (2H, br s), 5.22 (2H, br s), 4.77 (2H, s), 4.27 (2H, q, J 7.2 Hz), 2.40 (3H, s) and 1.32 (3H, t, J 7.2 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05922741 |
| Source dataset | uspto-grants-1999_07 |
| ORD ID | ord-ee0b6ada0b1645d7bc9014a9ca733bef |
| Source note | uspto-grants-1999_07 |