HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18354197, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 18354198 | HCID 18354198 | — |
| Reactant | HCID 22104197 | HCID 22104197 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 18354197 | HCID 18354197 | 89% |
Reaction Steps
0.75 g (0.0049 mol) of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) is added to a solution of 0.5 g (0.0019 mol) of 3-formylamino-2-pyridinesulfonamide and 0.68 g (0.0025 mol) of N-(4,6-dimethoxypyrimidin-2-yl)phenylcarbamate in 40 ml of acetonitrile. The solution is stirred for 16 hours at room temperature, 20 ml of water are subsequently added, and the pH is brought to 4 using 2-normal hydrochloric acid. The mixture is extracted with dichloromethane, the organic phase is dried over MgSO4, and n-heptane is added. Filtration gives 0.64 g (89% of theory) of N-[(4,6-dimethoxy-pyrimidin-2-yl)-aminocarbonyl]-3-formylamino-2-pyridinesulfonamide of melting point 172° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06316388B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-b4eaf252c1204b8cadb85345c49c0dc2 |
| Source note | uspto-grants-2001_11 |