HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium formate → HCID 18943538, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium formate | HCID 2723923 | — |
| Reactant | HCID 18943563 | HCID 18943563 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18943538 | HCID 18943538 | 84.7% |
Reaction Steps
Into a 500 ml round bottomed flask, the product from step (b) (17 g) and ammonium formate (17 g) in THF (250 ml) were added. To the nitrogen purged reaction mixture, 10% Pd—C (4 g) was added. The reaction mixture was stirred at reflux for 3 hours. The reaction mixture was allowed to cool to room temperature and filtered through celite. The filtrate was diluted with water (200 ml) and extracted with EtOAc (3×). The combined EtOAc extracts were washed with saturated NaHCO3, brine, dried over NaSO4, and solvent evaporated in vacuo to give the sub-title compound as an off-white solid (12.9 g). 1H NMR (300 MHz, DMSO-d6) δ 6.83-6.78 (m, 1H); 6.39-6.31 (m, 2H); 4.91 (s, 2H); 3.66-3.56 (m, 4H); 2.81-2.73 (m, 4H); MS: ESI (positive): 259 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09284277B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-170c79b15151413a8ff953d5b22a8cf7 |
| Source note | uspto-grants-2016_03 |