HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Methyl-(5-trimethylsilanylethynyl-pyridin-2-yl)-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Trimethylsilylacetylene | HCID 66111 | — |
| Reactant | 5-Bromo-N-methylpyridin-2-amine | HCID 15645663 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Cyclohexane | HCID 8078 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Methyl-(5-trimethylsilanylethynyl-pyridin-2-yl)-amine | HCID 66705950 | — |
Reaction Steps
The title compound is synthesized according to general procedure GP2 starting from 4.3 g (23.0 mmol) 5-bromo-2-methylamino-pyridine and 4.5 mL (32.2 mmol) 1-trimethylsilyl-ethyne using 134 mg (0.71 mmol) CuI, 601 mg (2.3 mmol) triphenylphosphine, 420 mg (0.60 mmol) PdCl2(PPh3)2 and 32 mL (101 mmol) triethylamine in 40 mL dry THF. For the work-up the reaction mixture is diluted with ethyl acetate and small amounts of cyclohexane, the organic phase is extracted with water and brine. The product is purified by chromatography on silica gel using a hexane/ethyl acetate gradient. Yield: 4.0 g (85%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916548B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-701d45a5837548c79ffd456007ac7470 |
| Source note | uspto-grants-2014_12 |