Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 6042928 | HCID 6042928 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 178469254 | HCID 178469254 | — |
Reaction Steps
(Z)-ethyl 3-amino-2-(ethoxycarbonylcarbamothioyl)but-2-enoate was dissolved in 30% aqueous triethyl amine and the reaction mixture stirred at 70° C. After 2 hours, the reaction mixture was cooled and neutralized with glacial acetic acid and the aqueous mixture extracted with EtOAc. The organic layer was washed with water, dried over Na2SO4 and concentrated under vacuum to give the desired product. 1H NMR (400 MHz, DMSO-d6): δ 12.54 (s, 1H), 11.85 (s, 1H), 4.21 (q, J=7.6 Hz, 2H), 2.03 (s, 3H), 1.24 (t. J=7.6 Hz, 3H); MS m/z 213.1 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09382277B2 |
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| Source dataset | uspto-grants-2016_07 |
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| ORD ID | ord-9a7bc410288c4f408bf7e4f0b6c91980 |
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| Source note | uspto-grants-2016_07 |
|---|