Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | 4-Bromo-3-methylbenzonitrile | HCID 2737494 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18475738 | HCID 18475738 | 11.5% |
Reaction Steps
To a solution of 4-bromo-3-methylbenzonitrile (11 g, 56 mmol) and potassium fluoride (3.3 g, 56 mmol) in anhydrous N,N-dimethylformamide (150 mL) was added morpholine (15 g, 170 mmol) and the reaction was heated at 145° C. for 4 days. The solvent was evaporated in vacuo and the residue was partitioned between diethyl ether and water. The phases was separated and the organic phase was dried (Na2SO4), filtered and evaporated in vacuo. Purification on a silica gel column using toluene followed by chloroform as eluents gave 1.3 g (11% yield) of the title compound as white crystals: mp 85-86° C.; EIMS (70 eV) m/z (relative intensity) 202 (71, M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06410530B1 |
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| Source dataset | uspto-grants-2002_06 |
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| ORD ID | ord-254af52978764d25a2291a29606e26f9 |
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| Source note | uspto-grants-2002_06 |
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