Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 4-Bromoaniline | HCID 7807 | — |
| Reactant | Ethyl 2-oxocyclopentanecarboxylate | HCID 69136 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67316421 | HCID 67316421 | — |
Reaction Steps
To a mixture of 4-bromoaniline (3.44 g) in 5M aqueous HCl (12 mL) at 0° C. was added 2.5M NaNO2 (1.38 g) in water (20 mL). After the addition, 4.5M sodium acetate (9.23 g) in water (25 mL) was added, followed by 2-oxo-cyclopentanecarboxylic acid ethyl ester (3 mL). The mixture was stirred at 0° C. for 15 minutes, warmed to 19° C. over two hours, and extracted with dichloromethane. The extract was dried (MgSO4), filtered and concentrated. The concentrate was dissolved in 10% H2SO4 in ethanol (22 mL) and refluxed overnight, cooled to room temperature, quenched with water (0.4 L), and filtered.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08853209B2 |
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| Source dataset | uspto-grants-2014_10 |
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| ORD ID | ord-badf0219465c45218d5f3ab92312e178 |
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| Source note | uspto-grants-2014_10 |
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