Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydrazinecarboxaldehyde | HCID 12229 | — |
| Reactant | Ethyl 4-bromobenzimidate hydrochloride | HCID 19017302 | — |
| Product | HCID 178419362 | HCID 178419362 | 48.3% |
Reaction Steps
Ethyl 4-bromobenzimidate hydrochloride (35.6 g, 135 mmol), formic hydrazide (16.16 g, 269 mmol) and triethylamine (75 mL, 538 mmol) were combined in a screw capped flask and heated to 85° C. for 16 h. The solution was condensed under reduced pressure to afford a solid, which was partitioned between water and ethyl acetate (3×), dried over magnesium sulfate and solvent removed under reduced pressure. The resulting solid was sonicated with 20% ethyl acetate in hexanes, filtered and dried to afford the title compound (14.6 g, 65.2 mmol, 48% yield). MS (ESI) m/z 224.1 [M]+, 226.1 [M+2]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08569494B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-13106086af0f434e86f05a50b0f14a08 |
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| Source note | uspto-grants-2013_10 |
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