Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 13086678 | HCID 13086678 | — |
| Reactant | HCID 86754833 | HCID 86754833 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178470743 | HCID 178470743 | 66.9% |
Reaction Steps
A mixture of 2.5 g of ethyl (ethylthio)iminoacetate tetrafluoroborate, 110 ml of acetic acid, 1.8 g of ethyl 4-aminoacetoacetate hydrochloride and 1.64 g of sodium acetate is heated for 3 hours at a temperature close to 95° C. The reaction mixture is filtered and the insoluble matter is rinsed with 3×5 ml of acetic acid. The filtrate is evaporated in a rotary evaporator and the evaporation residue is supplemented with 75 ml of dichloromethane. The organic solution is dried over sodium sulphate, filtered and evaporated in a rotary evaporator. The evaporation residue (1.86 g) is purified by chromatography on a silica column, eluting with ethyl acetate. 1.5 g of ethyl 4-(ethoxycarbonylmethyl)imidazole-2-carboxylate are obtained in the form of a red-yellow solid melting at 88° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05990108 |
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| Source dataset | uspto-grants-1999_11 |
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| ORD ID | ord-c963d74eb0ec4ee1af85520dbe8edcea |
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| Source note | uspto-grants-1999_11 |
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