反应详情

60% sodium hydride was added to 10 ml of a tetrahydrofuran suspension containing 1.00 g of trans-4-aminocyclohexanol hydrochloride and the mixture was refluxed for 1 hour. After cooling to room temperature, 2-chloropyrimidine was slowly added thereto and the mixture was stirred at room temperature for 6 hours. The reaction mixture was poured into ice-cold water and extracted with chloroform. The extract was washed with brine and dried over anhydrous sodium sulfate, and then, the solvent was removed under reduced pressure. The residue was purified by NH-silica gel column chromatography (solvent: ethyl acetate-hexane (1:4) to chloroform alone) to obtain 788 mg of trans-4-(2-pyrimidinyloxy)cyclohexylamine (Reference Example 9-46 in Table 6).

1. temperaturethe mixture was refluxed for 1 hour
2. additionThe reaction mixture was poured into ice-cold water
3. extractionextracted with chloroform
4. washThe extract was washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. customthe solvent was removed under reduced pressure
7. customThe residue was purified by NH-silica gel column chromatography (solvent