HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 5-(Azidomethyl)pyridine-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Methanesulfonate | HCID 85257 | — |
| Reactant | 2-Cyano-5-hydroxymethylpyridine | HCID 12251966 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-(Azidomethyl)pyridine-2-carbonitrile | HCID 21904627 | 83% |
Reaction Steps
5-(Hydroxymethyl)pyridine-2-carbonitrile (4 g, 0.03 mol; see step (ii) above) was dissolved in 25 mL of methylene chloride and cooled in an ice bath. Mesyl chloride (2.32 mL, 0.0300 mol) and then triethylamine (4.6 mL, 0.033 mol) were added dropwise. The reaction mixture was stirred and after work up the crude mesylate was treated with NaN3 (7.35 g, 0.113 mol) in 20 mL of DMF. The reaction mixture was stirred at 40° C. for 2 h, diluted with water and extracted with ethyl acetate. The organic layer was concentrated to yield 3.95 g (83%) of the crude azide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07645751B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-8c9ec290d5a04cfebf2432e7a135eeb7 |
| Source note | uspto-grants-2010_01 |