HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → Sulfamethizole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | N-(4-(((5-Methyl-1,3,4-thiadiazol-2-yl)amino)sulphonyl)phenyl)acetamide | HCID 791566 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | Sulfamethizole | HCID 5328 | 72.5% |
Reaction Steps
Compound 106 (250 mg, 0.8 mmol) was suspended in 3 N HCl (4 mL) and the suspension heated to reflux for 30 min. Following neutralization with saturated aqueous Na2CO3 solution, the precipitated product was collected by filtration, washed with water (3×20 mL), and dried under vacuum. The residue was crystallized from MeOH to give the product (155 mg, 0.58 mmol, 72%) as a solid, mp 207-208° C. (lit mp 208)1; 1H NMR (500 MHz, DMSO) δ 2.47 (3, s), 5.89 (2, s), 6.58 (2, d, J=8.5 Hz), 7.40 (2, d, J=8.5 Hz), 10.48 (1, s); 13C NMR (125 MHz, DMSO) δ 16.0, 112.5, 127.2, 127.6, 152.4, 153.6, 166.8.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08962663B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-34bb1545e18d4b45864f64523c904264 |
| Source note | uspto-grants-2015_02 |