HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-4-difluoromethoxy-3-dimethoxymethyl-1-fluorobenzene → 2-Chloro-6-difluoromethoxy-3-fluorobenzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-4-difluoromethoxy-3-dimethoxymethyl-1-fluorobenzene | HCID 67004363 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2-Chloro-6-difluoromethoxy-3-fluorobenzaldehyde | HCID 86659324 | 40% |
Reaction Steps
To a solution of crude 2-chloro-4-difluoromethoxy-3-dimethoxymethyl-1-fluorobenzene (181 g, 670 mmol) in acetone (650 mL) and water (150 mL) was added Amberlyst-15 resin (540 g, pre-washed with water) and the mixture was stirred using mechanical stirrer for 40 h at RT. The Amberlyst-15 resin was removed by filtration using celite bed on sintered funnel, and the filtrate was evaporated on a rotary evaporator at RT (Note: aldehyde evaporates at higher temperatures under reduced pressure). The residue was purified by column chromatography on silica gel using ethyl acetate/hexanes (5% to 10%) to obtain the title compound (60 g, 40%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08445510B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-0e5dd5fc9efe4cd7b3615ab8785f5da5 |
| Source note | uspto-grants-2013_05 |