HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Chlorobenzotrifluoride → HCID 6190431, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Chlorobenzotrifluoride | HCID 7374 | — |
| Reactant | Styrene | HCID 7501 | — |
| Reactant | Di-tert-butylphenylphosphine | HCID 316378 | — |
| Reactant | alpha-Cyclohexylcyclohexanemethanamine | HCID 10774245 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 6190431 | HCID 6190431 | — |
Reaction Steps
0.745 g (7.2 mmol) of styrene, 38.7 mg (120 μmol) of NBu4Br, 6.7 mg (30 μmol) of palladium acetate and 26.7 mg (120 μmol) of phenyldi(t-butyl)phosphine are weighed into a Schlenk vessel. 1.08 g (6 mmol) of 3-chlorobenzotrifluoride and 1.53 ml (7.2 mmol) of dicyclohexylmethylamine and also 3.5 ml of dimethylacetamide are then added. The Schlenk vessel is placed in a heating bath at 130° C. and the contents are stirred. After 4 hours, the contents are poured into 30 ml of water and the product is extracted by shaking with t-butyl methyl ether. After drying the organic phase over MgSO4, the solvent is removed under reduced pressure and the product is isolated. Yellowish, crystalline solid, yield: 1.43 g (96% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07102046B2 |
| Source dataset | uspto-grants-2006_09 |
| ORD ID | ord-c1fd83eb8b9f4ab6a3b234aad9580f6e |
| Source note | uspto-grants-2006_09 |