HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1-Bis(methylthio)-2-nitroethylene → HCID 178503826, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1-Bis(methylthio)-2-nitroethylene | HCID 83623 | — |
| Reactant | HCID 178433288 | HCID 178433288 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 178503826 | HCID 178503826 | 54.9% |
Reaction Steps
(a)(i) A solution of 4-methyl-5-[(2-aminoethyl)thiomethyl]-imidazole (1.71 g) in t-butanol (30 ml) was added slowly to a solution of 1-nitro-2,2-bis methylthioethylene (1.66 g) in acetonitrile (20 ml) at room temperature. The solution was heated under reflux for 3 hours, evaporated to dryness and chromatographed on a column of silica gel with elution by anhydrous ether (250 ml) followed by acetone (500 ml). The acetone eluate was concentrated to low bulk to give 1-nitro-2-methylthio-2-[2-((4-methyl-5-imidazolyl)methylthio)ethylamino]ethylene (1.58 g), m.p. 151°-153°. A sample recrystallised from acetonitrile had m.p. 152°-153°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04080459 |
| Source dataset | uspto-grants-1978_03 |
| ORD ID | ord-64d3cbd757864fd78d1db8880d683bcd |
| Source note | uspto-grants-1978_03 |