Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 10242642 | HCID 10242642 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67973797 | HCID 67973797 | 133.9% |
Reaction Steps
A mixture of ethyl 5-fluoro-1-oxo-indane-2-carboxylate (1.4 g, 6.3 mmol), sodium hydride (278 mg, 6.9 mmol, 60% in mineral oil) and DMF (dry, 2.5 ml) was heated to 65° C. for one hour. A solution of bromo ethylester (1.15 g, 0.8 ml, 6.9 mmol) in dry DMF (4.0 ml) was added at the same temperature and heating was continued for additional 3 h. After complete the reaction, reaction mass was evaporated to dryness, 5 ml water was added and the suspension was extracted with ethyl acetate (25 ml×3). Combined organic layer was washed with brine, dried over sodium sulphate, evaporated and subjected to column chromatography using ethyl acetate/hexane (15%) to yield a desired product (1.3 g, 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08946280B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-26d02dabfe1d48d8819f377992505f80 |
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| Source note | uspto-grants-2015_02 |
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