HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 86742014, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Epibromohydrin | HCID 18430 | — |
| Reactant | HCID 135617184 | HCID 135617184 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | HCID 86742014 | HCID 86742014 | — |
Reaction Steps
A mixture of 14 g of 3-(2-hydroxyphenyl)-1-methyl-1H-thieno[3,2-c]pyrazole, 10 g of epibromohydrin, 5 g of potassium carbonate and 75 ml of acetonitrile was stirred under nitrogen at 70°-80° C. After 16 hours of stirring, thin layer chromatography (1:1 hexane/ethyl acetate) showed residual starting material. Therefore, 2 g of epibromohydrin and 10 ml of dimethylformamide were added and the mixture was stirred overnight at 92° C., and thereafter quenched, extracted with ether/ethyl acetate (1:1), washed and dried (over anhydrous magnesium sulfate). The epoxide was separated from other by-products using HPLC (eluent=DCM).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04769472 |
| Source dataset | uspto-grants-1988_09 |
| ORD ID | ord-e1cfba41f49f41a5a617bffeea978a54 |
| Source note | uspto-grants-1988_09 |