Cesium carbonate → HCID 68313044、化合物
反応式
C(OC(N1CCC(C(O[C:21]2[CH:43]=[CH:42][C:24]3[C:25]4[N:29]([CH2:30][CH2:31][O:32][C:23]=3[CH:22]=2)[CH:28]=[C:27]([C:33]2[N:34]([CH:39]([CH3:41])[CH3:40])[N:35]=[C:36]([CH3:38])[N:37]=2)[N:26]=4)CC)CC1)=O)C1C=CC=CC=1.[CH2:44]([O:51][C:52]([N:54]1[CH2:59][CH2:58][CH:57]([CH:60]([O:65]S(C(F)(F)F)(=O)=O)[C:61]([F:64])([F:63])[F:62])[CH2:56][CH2:55]1)=[O:53])[C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[CH2:44]([O:51][C:52]([N:54]1[CH2:59][CH2:58][CH:57]([CH:60]([O:65][C:21]2[CH:43]=[CH:42][C:24]3[C:25]4[N:29]([CH2:30][CH2:31][O:32][C:23]=3[CH:22]=2)[CH:28]=[C:27]([C:33]2[N:34]([CH:39]([CH3:41])[CH3:40])[N:35]=[C:36]([CH3:38])[N:37]=2)[N:26]=4)[C:61]([F:64])([F:63])[F:62])[CH2:56][CH2:55]1)=[O:53])[C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1参加物
5
実験手順
2-(2-Isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-ol from Example 4 (300 mg, 0.92 mmol), 4-(2,2,2-trifluoro-1-trifluoromethanesulfonyloxyethyl)piperidine-1-carboxylic acid benzyl ester (870 mg, 2.1 mmol) and Cs2CO3 (680 mg, 2.1 mmol) were suspended in DMF (5 mL), stirred at RT for 2 h and then heated at 80° C. for 18 h. The reaction mixture was then quenched with water and extracted with EtOAc. The organic phase was washed with brine, dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by column chromatography (Si-PCC, gradient 0-10% MeOH in EtOAc) affording the title compound (210 mg, 37%). LCMS: RT 4.04 min [M+H]+ 625.0.