Triethylamine → HCID 46851730、化合物

反応式

[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([CH2:17][CH:18]4[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]4)(=[O:16])=[O:15])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH2:3][CH2:2]1.Cl.Cl[C:31]1[CH:36]=[CH:35][N:34]=[CH:33][CH:32]=1.C(N(CC)CC)C>C(O)C>[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([CH2:17][CH:18]4[CH2:19][CH2:20][N:21]([C:31]5[CH:36]=[CH:35][N:34]=[CH:33][CH:32]=5)[CH2:22][CH2:23]4)(=[O:15])=[O:16])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH2:2][CH2:3]1

参加物

反応条件

温度: 150 °C

実験手順

A mixture of 1-(cyclopropylmethyl)-2-neopentyl-5-(piperidin-4-ylmethylsulfonyl)-1H-benzo[d]imidazole (STEP D, 25 mg, 0.062 mmol), 4-chloropyridine hydrochloride (19 mg, 0.12 mmol) and triethylamine (35 microL, 0.25 mmol) in ethanol was stirred at 150° C. under microwave for 3 h. The solvent was removed. The residue was diluted with ethyl acetate and saturated sodium bicarbonate aqueous solution to separate. The aqueous layer was extracted with ethyl acetate (3 mL×2) and the organic layer was filtered through magnesium sulfate column. The filtrate was concentrated in vacuo. The residue was purified by prep-LC-MS (“process A”).