HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → Pyridine, 4,5-bis(chloromethyl)-2-(trifluoromethyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 6-(Trifluoromethyl)-3,4-pyridinedimethanol | HCID 58687922 | — |
| Product | Pyridine, 4,5-bis(chloromethyl)-2-(trifluoromethyl)- | HCID 57753353 | 66% |
Reaction Steps
To a room temperature suspension of 2.5 mmol (5-Hydroxymethyl-2-trifluoromethyl-pyridin-4-yl)-methanol (CAS: 765298-25-7) in 3 ml dichloromethane was added dropwise 12.5 mmol thionylchloride. After 1 hour, the reaction mixture was evaporated in vacuo. The residue was dissolved in dichloromethane and washed with saturated sodium bicarbonate solution, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by chromatography (SiO2, heptane/ethyl acetate) to yield the title compound as a light yellow oil (66% yield). MS (m/e): 243.0 (M−H, 100%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07557114B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-072a9ed33eb64a33bf047e4c9a85590f |
| Source note | uspto-grants-2009_07 |