HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178522902, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethynylpyridine | HCID 137268 | — |
| Reactant | HCID 178522917 | HCID 178522917 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178522902 | HCID 178522902 | 59.1% |
Reaction Steps
A solution of the title compound of Example 5 (540.3 mg), 2-ethynyl pyridine (0.172 g), PdCl2 (PPh3)2 (21.1 mg), and 0.75 mL Et3N in 3 mL DMF is heated at 90° C. for 1 hr. The reaction mixture is cooled to room temperature and diluted with H2O. A tan solid precipitates, which is collected, dissolved in a mixture of CH2Cl2 and MeOH, and adsorbed onto silica. The crude product is chromatographed eluting with 2% MeOH in CH2Cl2. Fractions homogenous by TLC are combined, condensed and recrystallized from hot MeOH/CH2Cl2 and hexanes to yield 0.302 g of the desired product as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06093732 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-8c6ef6a6fd73479895bce6a6c7d6b6b8 |
| Source note | uspto-grants-2000_07 |