HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Hydroxymethylpyridine → Ethyl 5-trifluoromethyl-1-[(pyrid-4-yl)methyl]-1H-indole-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Hydroxymethylpyridine | HCID 11472 | — |
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | Ethyl 5-(trifluoromethyl)-1H-indole-2-carboxylate | HCID 17389890 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Ethyl 5-trifluoromethyl-1-[(pyrid-4-yl)methyl]-1H-indole-2-carboxylate | HCID 68431838 | 77.5% |
Reaction Steps
A solution of 1.47 g (5.83 mmol) of 1,1′-(azodicarbonyl)dipiperidine in 50 ml of toluene is added dropwise to a solution of 1 g (3.89 mmol) of ethyl 5-trifluoromethyl-1H-indole-2-carboxylate, 0.63 g (5.83 mmol) of 4-pyridylcarbinol and 1.46 ml (5.83 mmol) of tributylphosphine in 50 ml of toluene. The reaction mixture is stirred overnight at room temperature and then concentrated under reduced pressure and chromatographed on a column of silica (eluent: dichloromethane/methanol). 1.05 g of expected product are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08318775B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-18f0bcb4503e486da3373a82a7b28c87 |
| Source note | uspto-grants-2012_11 |