HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylcarbamoyl Chloride → 2-(2,4-difluorophenyl)-3-(2-cyanopyridin-5-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | HCID 18956537 | HCID 18956537 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(2,4-difluorophenyl)-3-(2-cyanopyridin-5-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol | HCID 18956532 | 18.9% |
Reaction Steps
A mixture of the product of part (i) (0.93 g) and N,N-dimethylcarbamoyl chloride (0.40 g) in dichloromethane (10 ml) was stirred at room temperature overnight. Trimethylsilyl cyanide (0.40 g) was added and stirring was continued for a further 60 hours. The solution was washed with 10% sodium carbonate solution and the aqueous layer was separated and washed with dichloromethane. The organic layers were combined, dried (MgSO4) and evaporated. The residue was chromatographed on silica gel using hexane/isopropanol (4:1) as eluant to give 2-(2,4-difluorophenyl)-3-(2-cyanopyridin-5-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol, (0.18 g), m.p. 136°-141°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05206364 |
| Source dataset | uspto-grants-1993_04 |
| ORD ID | ord-cb068c2d9add44318a2c5531621420ff |
| Source note | uspto-grants-1993_04 |