HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → Ammonia
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Piperazin-1-yl-1,3-benzothiazole | HCID 592122 | — |
| Reactant | 2-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonate | HCID 86739600 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | Ammonia | HCID 222 | — |
| Product | 3-[4-(Benzothiazol-2-yl)-piperazin-1-yl]-2-(2,4-dichlorophenyl)-1-(1H-1,2,4-triazol-1-yl)propan-2-ol | HCID 19837958 | — |
Reaction Steps
A mixture of benzothiazol-2-yl-piperazine (0.4 g, 1.55 mmole), 2-(2,4-dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonate (see EP-A-44605) (0.57 g, 1.55 mmole) and potassium carbonate (2 g, 14 mmole) in dioxan (20 ml) was heated at reflux for 3 days. After cooling, the mixture was diluted with methylene chloride, the insoluble inorganic material removed by filtration and the filtrate concentrated under reduced pressure. The resulting oil was purified by flash chromatography on silica gel eluting with ether (93): ethanol (7): 0.88 ammonia solution (1) to yield the desired product as a foam, m.p. 68°-85° (0.34 g, 44%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04885294 |
| Source dataset | uspto-grants-1989_12 |
| ORD ID | ord-15213472cb0d41cda48800d7ff4e308f |
| Source note | uspto-grants-1989_12 |