HCID 59242670、化合物 → HCID 59242651、化合物
反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:15]=[N:16][C:17]([C:26]([F:29])([F:28])[F:27])=[C:18]([C:20]3[S:21][C:22]([Cl:25])=[CH:23][CH:24]=3)[CH:19]=2)[CH2:10][CH2:9]1)=O)(C)(C)C>CO>[Cl:25][C:22]1[S:21][C:20]([C:18]2[CH:19]=[C:14]([N:11]3[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]3)[N:15]=[N:16][C:17]=2[C:26]([F:29])([F:27])[F:28])=[CH:24][CH:23]=1参加物
3
試薬・触媒・溶媒 1
実験手順
To a solution of 4-[5-(5-chloro-thiophen-2-yl)-6-trifluoromethyl-pyridazin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester (D15) (0.114 g, 0.25 mmol) in methanol (10 ml) was added Amberlyst® 15 ion exchange resin, acidic form (4.1 mmol/g) (0.305 g, 1.25 mmol) and the reaction mixture was shaken at room temperature for 18 h. After this period, the mixture was filtered and then a saturated solution of ammonia in methanol was added. The mixture was shaken for 1 h, filtered and the filtrate evaporated in vacuo. The residue was then purified by column chromatography (silica gel; 3% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and evaporated in vacuo. The crude product was dissolved in a 2 M solution of hydrochoric acid in diethyl ether and the mixture stirred at room temperature for 16. The solvent was evaporated in vacuo. The solid obtained was triturated from diethyl ether to yield E27 (0.062 g, 87%). C13H12ClF3N4S requires 348; Found 349 (MH+).