HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 21437373, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | HCID 21437372 | HCID 21437372 | — |
| Solvent | Formic Acid | HCID 284 | — |
| Product | HCID 21437373 | HCID 21437373 | 66% |
Reaction Steps
225 parts of 2-octyl-5-nitroimidazole is boiled under reflux with 500 parts of formic acid and 126 parts of dimethyl sulfate for 4 hours, the formic acid is distilled off in vacuo and 500 parts of water is added to the residue. The unreacted 2-octyl-5-nitroimidazole (72 parts) is separated and the aqueous phase is adjusted with aqueous ammonia solution to pH 10 so that the 1-methyl-2-octyl-5-nitroimidazole separates as an oily substance. The crude product is dissolved in ether and saturated with hydrogen chloride while cooling. 123 parts of 1-methyl-2-octyl-5-nitroimidazole having a melting point of 141° C. is obtained and this is equivalent to a yield of 66% of theory based on the 2-octyl-5-nitroimidazole reacted.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04021442 |
| Source dataset | uspto-grants-1977_05 |
| ORD ID | ord-8dc3c678d9dd4050b0cbb820ff4aa591 |
| Source note | uspto-grants-1977_05 |