Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl iodoacetate | HCID 12183 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178418311 | HCID 178418311 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 895571-94-5 | HCID 42643123 | — |
Reaction Steps
61.1 To a stirred mixture of 2.8 g 3-amino-1,2,4-triazole in 50 ml DMF, 1.57 g NaH were slowly added at 0° C. under an argon atmosphere. After 1 hr stirring at 0° C., 3.31 ml ethyliodoacetate were added. The reaction mixture was stirred at r.t. over night. The mixture was diluted with water and extracted with EtOAc and CH2Cl2/MeOH 9:1. The organic phase was dried (MgSO4), filtered and concentrated. The crude product was purified by chromatography on silica, using a gradient from CH2Cl2 to CH2Cl2/MeOH 9:1 and then crystallization from cyclohexane/EtOAc to give 750 mg (3-amino-[1,2,4]triazol-1-yl)-acetic acid ethyl ester as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07361672B2 |
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| Source dataset | uspto-grants-2008_04 |
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| ORD ID | ord-07e78817063e4d9085e5cba8e9c4cbfa |
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| Source note | uspto-grants-2008_04 |
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