Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetylthiourea | HCID 2723593 | — |
| Reactant | HCID 22282466 | HCID 22282466 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22282502 | HCID 22282502 | 30.2% |
Reaction Steps
To a solution of methyl 2-bromo-3-(3-cyanophenyl)-3-oxopropionate (1.25 g, 4.4 mmol) in 20 mL of tetrahydrofuran was added 1-acetylthiourea (0.52 g, 4.4 mmol). The resulting mixture was stirred at 65° C. for 3 h. The reaction was allowed to cool and the solvent was evaporated in vacuo. The residue was taken up in ethyl acetate, washed with 10% aq HCl, saturated aq NaHCO3 and brine, dried (MgSO4) and concentrated in vacuo to yield a solid. Trituration with hexanes/ethyl acetate left the title compound as a white solid (0.4 g, 30%). MS (ESI) 302.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06962935B2 |
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| Source dataset | uspto-grants-2005_11 |
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| ORD ID | ord-314fe02a73b74a39935da5a5bae52473 |
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| Source note | uspto-grants-2005_11 |
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