Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | HCID 90303209 | HCID 90303209 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 90303417 | HCID 90303417 | — |
Reaction Steps
A mixture of 2-bromo-3-oxocyclopentanecarbonitrile (crude from A.1.7.1.; ca. 13 g) and thiourea (13.77 g, 181 mmol) in dioxane (600 mL) was stirred at 80° C. for 1 h. The mixture was allowed to cool to RT, quenched with aq. sat. NaHCO3 and extracted with EtOAc. The comb. org. layers were washed with brine, dried over MgSO4, and conc. in vacuo. Purification by means of CC (2-20% MeOH (0.5% Et3N)/DCM) provided a brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09388197B2 |
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| Source dataset | uspto-grants-2016_07 |
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| ORD ID | ord-0e84cec31e204c1eaa9c90c12ec2bf02 |
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| Source note | uspto-grants-2016_07 |
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