反应详情

In the mixed solvent of 5 ml of ethanol and 4 ml of tetrahydrofuran were dissolved 168 mg of N-tert-butoxycarbonyl-trans-4-[(6-chloro-3-pyridazinyl)amino]cyclohexylamine (Reference Example 3-46) and 0.5 ml of triethylamine. To the solution was added 50 mg of 10% palladium carbon and the mixture was stirred under hydrogen atmosphere with normal pressure at room temperature for 1 day. After the catalyst was removed by filtration, the solvent was removed, and the residue was stirred in 2 ml of trifluoroacetic acid for 3 hours. The solvent was removed, an aqueous 10% sodium hydroxide solution was added to the residue, the mixture was extracted with chloroform and dried over anhydrous sodium sulfate. Subsequently, the solvent was removed under reduced pressure to obtain 61 mg of trans-4-(pyridazin-3-ylamino)cyclohexylamine (Reference Example 3-48 in Table 5).

1. customAfter the catalyst was removed by filtration
2. customthe solvent was removed
3. stirringthe residue was stirred in 2 ml of trifluoroacetic acid for 3 hours
4. customThe solvent was removed
5. additionan aqueous 10% sodium hydroxide solution was added to the residue
6. extractionthe mixture was extracted with chloroform
7. dry with materialdried over anhydrous sodium sulfate
8. customSubsequently, the solvent was removed under reduced pressure