Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Bromide | HCID 6332 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 18765173 | HCID 18765173 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18765170 | HCID 18765170 | 39% |
Reaction Steps
To a solution of the product of step (a) (6.95 g, 21.7 mmol) and bromoethane (1.78 ml, 23.8 mmol) in DMF (70 ml) was added potassium carbonate (4.49 g, 32.5 mmol) and the reaction was heated to 60° C. for 18 h. After cooling, the reaction mixture was partitioned between 2N aqueous HCl and EtOAc, the organic layer was separated, washed with H2O, dried over MgSO4 and evaporated. The crude product was purified on silica gel, eluting with CH2Cl2/MeOH (97/3, v/v) to afford the subtitle compound as a colourless solid (2.94 g, 39%). Rf 0.68 (CH2Cl2/MeOH 95/5, v/v). MS m/z 366 (MNH4+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06521629B2 |
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| Source dataset | uspto-grants-2003_02 |
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| ORD ID | ord-9839095905e94c64848f4e989c159207 |
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| Source note | uspto-grants-2003_02 |
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