Trifluoroacetic acid → (4-Cyclohexyl-piperidin-4-ylmethyl)-thiazol-2-yl-amine
反応式
FC(F)(F)C(O)=O.C(Cl)Cl.O.C(OC([N:19]1[CH2:24][CH2:23][C:22]([CH:32]2[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]2)([CH2:25][NH:26][C:27]2[S:28][CH:29]=[CH:30][N:31]=2)[CH2:21][CH2:20]1)=O)(C)(C)C.FC(F)(F)C(O)=O>>[CH:32]1([C:22]2([CH2:25][NH:26][C:27]3[S:28][CH:29]=[CH:30][N:31]=3)[CH2:21][CH2:20][NH:19][CH2:24][CH2:23]2)[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37]1参加物
4
実験手順
A ready-to-use solution of trifluoroacetic acid:methylene chloride:water (1:1:0.1, 7 mL) is added to 4-cyclohexyl-4-(thiazol-2-ylaminomethyl)-piperidine-1-carboxylic acid tert-butyl ester, 12, (312 mg, 0.82 mmol), and the reaction mixture is stirred for 0.5–1.0 hour. The mixture is then concentrated under reduced pressure and partitioned between aqueous sodium bicarbonate and ethyl acetate. The organics are separated and the solvent removed under reduced pressure. The crude product is purified by preparative HPLC to afford 220 mg (96% yield) of the desired compound as the trifluoroacetic acid salt.