HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → 1-[(2-Methylquinolin-5-yl)amino]-4,4-dimethyl-2-(trifluoromethyl)-1,2,3,4-tetrahydronaphthalen-2-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1,1,1-Trifluoro-4-phenyl-2-[(2-methylquinolin-5-yl)iminomethyl]-4-methylpentan-2-ol | HCID 17989165 | — |
| Catalyst | titanium tetrachloride CH2Cl2 | HCID 57473882 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-[(2-Methylquinolin-5-yl)amino]-4,4-dimethyl-2-(trifluoromethyl)-1,2,3,4-tetrahydronaphthalen-2-ol | HCID 68682359 | 84.7% |
Reaction Steps
5.1 ml of a 1 M titanium tetrachloride-CH2Cl2 solution is added in drops to a solution of 111 mg of 1,1,1-trifluoro-4-phenyl-2-[(2-methylquinolin-5-yl)iminomethyl]-4-methylpentan-2-ol in 84 ml of CH2Cl2 at −78° C. After 1 hour at −78° C., the batch is mixed with saturated NaHCO3 and heated to room temperature. The phases are separated, the aqueous phase is extracted with CH2Cl2, the combined organic phases are dried (Na2SO4) and concentrated by evaporation in a vacuum. Column chromatography on silica gel with cyclohexane-ethyl acetate yields 94 mg of product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07659297B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-8e1a3a019a994d19b7638bbb622f72a7 |
| Source note | uspto-grants-2010_02 |