Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | 3,4-Difluorobenzaldehyde | HCID 588088 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 16790478 | HCID 16790478 | — |
Reaction Steps
Through a solution of 3,4-difluorobenzaldehyde (25.0 g, 0.176 mol) in MeOH (500 mL) in a round bottom flask, was bubbled ammonia gas for two hours at room temperature. The flask was then cooled to 0° C. and trimethylsilyl cyanide was then added slowly. The reaction mixture was stirred for 2 h, at which time TLC analysis indicated that the reaction was complete (Rf=0.35, 3:2 hexane/EtOAc). The solvent was removed in vacuo and the residue was subjected to flash column chromatography on silica gel to obtain the desired product, which was used in the next step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06727264B1 |
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| Source dataset | uspto-grants-2004_04 |
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| ORD ID | ord-26eb8c4a49ec4c398b26c834d3071124 |
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| Source note | uspto-grants-2004_04 |
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