HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyanoacetamide → HCID 58056952, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyanoacetamide | HCID 7898 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl 4-fluoro-3-nitrobenzoate | HCID 5219721 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58056952 | HCID 58056952 | 68% |
Reaction Steps
Starting material 25 (10 g, 50 mmol) and cyanacetamide (26, 8.4 g, 100 mmol) were dissolved in dry THF and NaH (60% ig, 4 g, 100 mmol) was added. The reaction was stirred over night at ambient temperature. Now it was cooled to 0° C. and 4 N HCl/Dioxan was added. The reaction mixture was concentrated in vacuo, the solid residue crystallized with 400 ml isopropyl ethyl ether, resulting crystals were filtered and dried. Then the crystals were washed with water and again filtered and dried. Thereby 8.9 g of the desired product 27 (67%, 34 mmol) were isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08497283B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-48946bbb0b774c688aca42a64732e121 |
| Source note | uspto-grants-2013_07 |