HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-Bis(trifluoromethyl)benzyl bromide → N-(3,5-Bis-trifluoromethyl-benzyl)-N-methyl-6-morpholin-4-yl-4-o-tolyl-nicotinamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-Bis(trifluoromethyl)benzyl bromide | HCID 122573 | — |
| Reactant | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| Reactant | N-methyl-6-morpholin-4-yl-4-o-tolyl-nicotinamide | HCID 22479279 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-(3,5-Bis-trifluoromethyl-benzyl)-N-methyl-6-morpholin-4-yl-4-o-tolyl-nicotinamide | HCID 10119544 | 44% |
Reaction Steps
To a solution of 0.27 g (0.87 mmol) N-methyl-6-morpholin-4-yl-4-o-tolyl-nicotinamide in 15 ml tetrahydrofuran, 1.12 ml of a 1 M solution (1.12 mmol) of potassium hexamethyldisilazide in tetrahydrofuran was added at 0° C. After 30 min, 0.16 ml (0.87 mmol) 3,5-bis(trifluoromethyl)benzyl bromide were added dropwise and the reaction mixture was allowed to warm to room temperature over night. Quenching with water was followed by extraction with ethyl acetate. The combined organic extracts were dried with sodium sulfate and concentrated. Column chromatography gave 0.20 g (44%) of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06806370B2 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-896fcd5b235542c6852ef646485e65d7 |
| Source note | uspto-grants-2004_10 |