HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclopropyl isothiocyanate → 3-Cyclopropyl-1-[2-(5-fluoro-pyridin-3-yl)-4-methyl-thiazol-5-yl]-1-methyl-thiourea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclopropyl isothiocyanate | HCID 92463 | — |
| Reactant | 2-(5-fluoropyridin-3-yl)-N,4-dimethylthiazol-5-amine | HCID 66645341 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 3-Cyclopropyl-1-[2-(5-fluoro-pyridin-3-yl)-4-methyl-thiazol-5-yl]-1-methyl-thiourea | HCID 59580497 | 73% |
Reaction Steps
A solution of 2-(5-fluoropyridin-3-yl)-N,4-dimethylthiazol-5-amine (200 mg, 0.896 mmol) and isothiocyanatocyclopropane (266 mg, 2.69 mmol) in dioxane (10 mL) was heated at 100° C. for 24 h before the solvent was removed under reduced pressure. The residue was purified via silica gel chromatography (0 to 100% ethyl acetate/hexanes) to afford the title compound as a yellow solid (211 mg, 73%): mp 117-119° C.; 1H NMR (400 MHz, CDCl3) δ 8.89 (s, 1H), 8.56 (d, J=2.8 Hz, 1H), 7.96 (dt, J=9.2 Hz, 2.4 Hz, 1H), 5.91 (br s, 1H), 3.62 (s, 3H), 3.04-2.99 (m, 1H), 2.31 (s, 3H), 0.89-0.81 (m, 2H), 0.57-0.48 (m, 2H); ESIMS m/z 323 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08350044B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-4641702f6cdc4ae392fbada8e38f2d6e |
| Source note | uspto-grants-2013_01 |