HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanone, 1-(1-methyl-1H-1,2,4-triazol-3-yl)- (9CI) → HCID 86669574, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanone, 1-(1-methyl-1H-1,2,4-triazol-3-yl)- (9CI) | HCID 14978352 | — |
| Reactant | HCID 178418486 | HCID 178418486 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86669574 | HCID 86669574 | — |
Reaction Steps
To a solution of ethynylmagnesium bromide (0.5M in THF, 4.32 mL, 2.16 mmol) at 0° C. was added 1-(1-methyl-1,2,4-triazol-3-yl)ethanone (180 mg, 1.44 mmol) in THF (5 mL) slowly. The reaction mixture was allowed to warm to RT and stirred for a further 1.5 hr. The reaction mixture was quenched with saturated aqueous NH4Cl solution (10 mL) and the organics were removed in vacuo. The product was extracted into EtOAc (×2) and the combined organics were dried (Na2SO4), filtered and concentrated in vacuo. Purification by column chromatography eluting with 2-10% methanol in DCM afforded the title compound: 1H NMR (500 MHz, CDCl3) delta 1.93 (3H, s), 2.62 (1H, s), 3.53 (1H, s), 3.93 (3H, s), 8.01 (1H, s); LC-MS: m/z=+152.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901313B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-f639fbe3400141b3ae1be4e5018b2df3 |
| Source note | uspto-grants-2014_12 |