反应详情

A 4-neck flask equipped with a reflux condenser was charged with 2-amino-1-(tetrahydropyran-4-yl)amino-4-trifluoromethylbenzene (see Synthesis Example 4) (0.62 g, 2.38 mmol) and anhydrous 1,4-dioxane (8.5 mL) and this was refluxed. Methoxyacetyl chloride (0.57 g, 5.25 mmol) in 1,4-dioxane solution (approx. 1.5 mL) was added dropwise to this over approximately 10 m. This was stirred under these conditions for 2 hours. This was allowed to cool, distilled water was added, and the solvent was distilled off under reduced pressure. This was successively extracted with t-butyl methyl ether, washed with brine, and dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure to yield the title compound (0.58 g, 77.4% yield) as a white powder.

1. customA 4-neck flask equipped with a reflux condenser
2. temperaturethis was refluxed
3. temperatureto cool
4. distillationdistilled water
5. additionwas added
6. distillationthe solvent was distilled off under reduced pressure
7. extractionThis was successively extracted with t-butyl methyl ether
8. washwashed with brine
9. dry with materialdried over anhydrous sodium sulfate
10. distillationthe solvent was distilled off under reduced pressure