Trifluoroacetic acid → (S)-N-(5-azaspiro[2.4]heptan-6-ylmethyl)-5-chloropyridin-2-amine
反応式
C(OC([N:8]1[C@H:14]([CH2:15][NH:16][C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][N:18]=2)[CH2:13][C:10]2([CH2:12][CH2:11]2)[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH2:11]1[C:10]2([CH2:13][C@@H:14]([CH2:15][NH:16][C:17]3[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][N:18]=3)[NH:8][CH2:9]2)[CH2:12]1参加物
4
反応条件
- 温度
- 0 °C
実験手順
(S)-tert-butyl6-(((5-chloropyridin-2-yl)amino)methyl)-5-azaspiro[2.4]heptane-5-carboxylate Intermediate 60, 600 mg, 1.77 mmol) was dissolved in dichloromethane (10 ml) and cooled to 0° C., then trifluoroacetic acid (4 ml) was added. After 1 hour at 0° C. and 3 hours at room temperature the solution was evaporated, the residue re-dissolved in dichloromethane was washed with saturated NaHCO3 aqueous solution. The organic layers were dried (Na2SO4) and concentrated under vacuum. The crude was purified by silica gel column chromatography (CHCl3/MeOH=8/2). (S)—N-(5-azaspiro[2.4]heptan-6-ylmethyl)-5-chloropyridin-2-amine was obtained as light yellow oil (400 mg).