HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 3-Amino-6-(trifluoromethyl)picolinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 2-Iodo-6-(trifluoromethyl)pyridin-3-amine | HCID 53425479 | — |
| Catalyst | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Product | 3-Amino-6-(trifluoromethyl)picolinonitrile | HCID 57364517 | 86.31% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
12.5 g (0.434 mol, 1 eq) of 5-amino-6-iodo-2-(trifluoromethyl)pyridine was dissolved in 125 mL of dry DMF and degasified with nitrogen for 5 min. 6.1 g (0.519 mol, 1.2 eq) of zinc cyanide and 5 g (0.1 eq) of Pd(PPh3)4 were added and heated at 100° C. for over night. The reaction mixture was quenched with water and extracted with ethyl acetate. The organic layer was washed with brine and concentrated. The crude product obtained was purified by 60-120 silica gel using 15% of ethyl acetate in pet ether to get 7 g (86.31%) of pale yellow solid. 1H NMR (CDCl3, 400 MHz): 4.85 (2H, bs), 7.25 (1H, d), 7.62 (1H, d). MS 188 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07985861B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-9aac442e773a4c3ba7ea6a548f044550 |
| Source note | uspto-grants-2011_07 |