HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 86589862, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 69039095 | HCID 69039095 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 86589862 | HCID 86589862 | — |
Reaction Steps
To a suspension of N-[1-(3,4-dichloro-phenyl)-1H-imidazol-4-ylmethyl]-acetamide (1.1 g, 3.7 mmol) in 1,2 dimethoxyethane (11 ml) was added Lawesson's reagent (0.82 g, 2.0 mmol) and the mixture refluxed for 90 min. After addition of saturated NaHCO3 solution (50 ml) and extraction with CH2Cl2 (3×100 ml) the combined organic phases were dried (Na2SO4), concentrated and the obtained crude product was chromatographed [silica, elution with gradient CH2Cl2 to 100% (CH2Cl2/MeOH=9:1)]. The title compound was obtained as a brown crystalline material (0.75 g, 68%). Mp. 166-170° C. (MeOH/CH2Cl2), MS: m/e=299 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06667335B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-7a56bedb151142f99bb711e80f173b0e |
| Source note | uspto-grants-2003_12 |