HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → N-[6-chloro-5-(2-chloro-5-methoxy-phenoxy)-pyrimidin-4-yl]-5-isopropyl-pyridine-sulphonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | 5-Isopropylpyridine-2-sulfonamide | HCID 18184193 | — |
| Reactant | 4,6-Dichloro-5-(2-chloro-5-methoxy-phenoxy)-pyrimidine | HCID 21979566 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | N-[6-chloro-5-(2-chloro-5-methoxy-phenoxy)-pyrimidin-4-yl]-5-isopropyl-pyridine-sulphonamide | HCID 18938912 | 53.2% |
Reaction Steps
306 mg of 4,6-dichloro-5-(2-chloro-5-methoxy-phenoxy)-pyrimidine, 320 mg of 5-isopropyl-2-pyridine-sulphonamide and 180 mg of K tert.butylate dissolved in 2 ml of DMSO were reacted at 90° C. for 3 hours. After cooling to room temperature the reaction medium was acidified with aqueous citric acid; the compound was extracted with ethyl acetate and, after distillation of the solvent, crystallized from ethanol. 250 mg of N-[6-chloro-5-(2-chloro-5-methoxy-phenoxy)-pyrimidin-4-yl]-5-isopropyl-pyridine-sulphonamide were obtained as white crystals with m.p. 174°-175° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05837708 |
| Source dataset | uspto-grants-1998_11 |
| ORD ID | ord-a64f9edbf272448ca2eee8ddd7ecc751 |
| Source note | uspto-grants-1998_11 |