HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13488631, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 13488624 | HCID 13488624 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 13488631 | HCID 13488631 | — |
Reaction Steps
To a suspension of 0.8 g NaH 80% in 25 ml DMF are added dropwise, at room temperature, a solution of 7.64 g 2-(4-chlorophenyl)-3-cyclopropyl-3-methyl-1-(1H-1,2,4-triazol-1-yl)-butan-2-ol in 50 ml DMF. The reaction is stirred at 40° for 30 minutes. Then are added dropwise, at 50°, 3.76 g CH3I. The mixture is stirred for 18 hours at 20°, then poured into one liter of water and extracted with CH2Cl2. The organic phases are washed with water, dried over MgSO4 and concentrated by continuous flask evaporation. The title compound is then obtained by chromatography of the residue on silica gel (mobile phase diethylether/triethylamine 10:2) in the form of white crystals, m.p. 87°-89°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04664696 |
| Source dataset | uspto-grants-1987_05 |
| ORD ID | ord-d4ebc9c411554a6b84a1961f240a4a82 |
| Source note | uspto-grants-1987_05 |