Trifluoroacetic acid → HCID 66773665、化合物
反応式
C(O)(C(F)(F)F)=O.C(OC([N:15]1[CH2:19][C:18]([F:21])([F:20])[CH2:17][C@H:16]1[CH2:22][NH:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([Cl:30])[CH:25]=1)=O)(C)(C)C>C(Cl)Cl>[Cl:30][C:26]1[CH:25]=[C:24]([NH:23][CH2:22][C@@H:16]2[CH2:17][C:18]([F:21])([F:20])[CH2:19][NH:15]2)[CH:29]=[CH:28][CH:27]=1参加物
4
実験手順
TFA (1 mL) was added to the solution of (S)-2-[(3-chloro-phenylamino)-methyl]-4,4-difluoro-pyrrolidine-1-carboxylic acid tert-butyl ester (0.16 g, 0.0004 mol) in DCM (5 mL) at 0° C. and the reaction mixture was stirred at rt for 12 h. The reaction was monitored by TLC. After completion, the reaction mixture was concentrated under reduced pressure using a rotary evaporator and washed with ether (3×10 mL). The crude was basified with sodium bicarbonate and the aqueous layer was extracted with DCM (3×50 mL). The organic layer was dried over anhydrous Na2SO4 and distilled using a rotary evaporator to give the desired (3-chloro-phenyl)-((S)-4,4-difluoro-pyrrolidin-2-ylmethyl)-amine (0.1 g) as a sticky solid.