HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 2-ethoxyethylidene-cyanoacetate → HCID 21076915, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 2-ethoxyethylidene-cyanoacetate | HCID 57299996 | — |
| Reactant | HCID 178448380 | HCID 178448380 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21076915 | HCID 21076915 | 44% |
Reaction Steps
To a stirred solution of [(R)-1-(N-Benzyl-carbamimidoyl)-2-methyl-propyl]-carbamic acid t-butyl ester (14.16 g, 46 mMol) in EtOH (50 mL) was added Ethyl 2-ethoxyethylidene-cyanoacetate (8.4 g, 46 mMol). The reaction was refluxed for 18 h, cooled to RT and concentrated under vacuum. Purification by flash chromatography on silica gel (5% EtOAc, CH2Cl2) followed by crystallization from EtOAc, hexane and Et2O, pet. ether gave the title compound (8.03 g, 44%) as a white solid: MS (ES) m/e 397.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07482343B2 |
| Source dataset | uspto-grants-2009_01 |
| ORD ID | ord-a8d4ed5cbc0c42d490b30a80d86c4171 |
| Source note | uspto-grants-2009_01 |