Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 19823379 | HCID 19823379 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86745031 | HCID 86745031 | — |
Reaction Steps
Acetic acid is added to a solution of ethyl 4-(2-formylamino-ethylthio)-3-oxo-butanoate (12.5 g) in MeOH (ml 120), previously saturated with ammonia at 0° C. and cooled at 0° C., up to pH 4-45. The mixture is refluxed for 2 hours and the excess solvent is evaporated in vacuum, to give a syrup from which a solid material is separated by treatment with AcOEt. After filtration, the organic phase is washed with water (8×10 ml), and with a saturated aqueous solution of NaHCO3 (3×10 ml), dried (Na2SO4) and concentrated in vacuum to give 11,5 g of ethyl 3-amino-4-(2-formylaminoethylthio)crotonate as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05047414 |
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| Source dataset | uspto-grants-1991_09 |
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| ORD ID | ord-a15a9f55509149ffa5080d6ad5072059 |
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| Source note | uspto-grants-1991_09 |
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