HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Formate → HCID 59799040, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Formate | HCID 2723810 | — |
| Reactant | HCID 57447750 | HCID 57447750 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59799040 | HCID 59799040 | 68% |
Reaction Steps
Mix 7-acetyl-9-bromo-6-hydroxy-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (833 mg, 2.2 mmol), tetrakis(triphenylphosphine)palladium(0) (150 mg, 0.13 mmol) and sodium formate (224 mg, 3.3 mmol) in anhydrous DMF (15 mL). Degas twice then flush with argon. Keep the flask under argon and heat the reaction at 95° C. for 16 h. Dilute with EtOAc then wash with 1 N HCl. Separate the organic layer, dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with 1:100 to 20:80 EtOAc:hexanes) to give the title compound (448 mg, 68%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981882B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-9471506e2b3f4276b41cacd3a92e59c8 |
| Source note | uspto-grants-2011_07 |