HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Anisoyl chloride → 3-methoxy-N-methyl-N-(4-(pyridin-2-yl)but-3-ynyl)benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Anisoyl chloride | HCID 74374 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | N-methyl-4-(pyridin-2-yl)but-3-yn-1-amine | HCID 66598286 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-methoxy-N-methyl-N-(4-(pyridin-2-yl)but-3-ynyl)benzamide | HCID 66598269 | 63.6% |
Reaction Steps
N-Methyl-4-(pyridin-2-yl)but-3-yn-1-amine (50 mg, 0.31 mmol) was dissolved in DCM (2 mL) and DIEA (67 μl, 0.41 mmol) was added at room temperature. The resulting mixture was cooled to 0° C. before the addition of 3-methoxybenzoyl chloride (69 mg, 0.41 mmol). After stirring overnight at room temperature, the mixture was quenched with water and extracted with DCM. DCM fractions were washed with water (10 mL), NaHCO3 sat (2*10 mL), water (10 mL), brine (10 mL). The solvent was removed and the crude residue was purified over silicagel chromatography (prepacked 10 g silicagel column, DCM/MeOH: from 100/0 to 95/5 as eluent) to afford 58 mg of 3-methoxy-N-methyl-N-(4-(pyridin-2-yl)but-3-ynyl)benzamide (Yield: 63%) as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08883826B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-bd6d29975b1346ed9a165b9126d5d440 |
| Source note | uspto-grants-2014_11 |