HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thionyl Chloride → HCID 178509689, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 178509719 | HCID 178509719 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178509689 | HCID 178509689 | 21.4% |
Reaction Steps
7.24 g of crude 4-[1-hydroxycyclohex-1-yl-1-(1,2,4-triazolyl)methyl]benzonitrile is dissolved at 0° in 50 ml of dichloromethane and stirred for 1 hour at 0° with 22.7 ml of thionyl chloride. Then the mixture is concentrated to dryness under vacuum, dissolved in 50 ml of dichloromethane, stirred with 30 ml of triethylamine for 2 hours, diluted with water, extracted four times with ethyl acetate, washed with sodium chloride solution, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, yielding 1.45 g of 4-[1-cyclohexylidene-1-(1,2,4-triazolyl)methyl]benzonitrile as a free base, mp 92°-93°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05411982 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-01e62add86ea4716b0053a88f5231ec4 |
| Source note | uspto-grants-1995_05 |