HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethyl orthoformate → 3-Chloro-2-(4-chloro-3-dimethoxymethylphenyl)-5-trifluoromethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | 2-Chloro-5-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]benzaldehyde | HCID 18692932 | — |
| Reactant | Bentonite | HCID 71586775 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Chloro-2-(4-chloro-3-dimethoxymethylphenyl)-5-trifluoromethylpyridine | HCID 19068745 | — |
Reaction Steps
50 ml of trimethyl orthoformate were added to 40.0 g of montmorillonite K-10 in 250 ml of anhydrous dichloromethane, after which a solution of 20.0 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine in 50 ml of dichloromethane was added dropwise while stirring and cooling in ice. After stirring at 23° C. for 20 hours, the clay was removed and thoroughly washed with dichloromethane. The dichloromethane phase was concentrated. The residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1). Yield: 22.1 g (96%) of a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05783522 |
| Source dataset | uspto-grants-1998_07 |
| ORD ID | ord-0ffccac45b144b839e75b0fdf07c86d6 |
| Source note | uspto-grants-1998_07 |