HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Nitrite → HCID 178515102, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Reactant | 6,11-dihydro-5H-dipyrido[2,3-b:4',3'-f]azepin-5-one | HCID 54759145 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178515102 | HCID 178515102 | 87% |
Reaction Steps
A solution of sodium nitrite (3.3 g, 0.048 mol) in water (14.4 mL) was added dropwise to a solution of 6,11-dihydro-5H-dipyrido[2,3-b:4′,3′-f]azepin-5-one (4.22 g, 0.02 mol) in acetic acid (80 mL) at room temperature. After the addition was completed, the reaction was stirred for 1.5 hours and 100 mL of water was then added. The mixture was stirred for additional 10 minutes, filtered and dried to give 4.18 g of the desired product. 1H NMR (400 MHz, CD3OD): δ 8.70 (s, 1H), 8.48-8.51 (m, 2H), 8.32 (d, 1H, J=5.2 Hz), 7.56 (d, 1H, J=5.6 Hz), 7.07 (dd, 1H, J1=8 Hz, J2=4.8 Hz). MS [M+H]=241.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08563541B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-15b3be77e53b45b2b84d3fef6f2ae04a |
| Source note | uspto-grants-2013_10 |