HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 66733743, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | HCID 66734199 | HCID 66734199 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Catalyst | Zinc bromide | HCID 10421208 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66733743 | HCID 66733743 | — |
Reaction Steps
A mixture of 3-(4-chloro-3,5-difluoro-phenyl)-acrylic acid butyl ester (5.000 g; 18.202 mmol), zinc bromide (0.819 g; 3.640 mmol), and 10% palladium over activated charcoal (0.320 g) was placed under nitrogen before EA (140 ml) was added. The resulting suspension was placed under vacuum, then under hydrogen (1 atm), and the reaction mixture was vigorously stirred at rt for 22 h. The reaction mixture was filtered over a pad of celite, and concentrated under reduced pressure to give the expected product 3-(4-chloro-3,5-difluoro-phenyl)-propionic acid butyl ester as a slightly yellow oil which was further dried under HV (5.020 g; 98%). LC-MS: tR=1.14 min.; [M+H]+: no ionisation.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188082B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-6ccca8724b494eb79d2f2758af0b9250 |
| Source note | uspto-grants-2012_05 |