5-Methyl-2-(1-methyl-piperidin-4-yl)-2H-pyrazol-3-ylamine → HCID 68078649, 화합물
반응식
[CH3:1][C:2]1[CH:6]=[C:5]([NH2:7])[N:4]([CH:8]2[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]2)[N:3]=1.[CH:15]1([C:18](=O)[CH2:19][C:20](=O)[C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:17][CH2:16]1>C1(C)C=CC=CC=1>[CH:15]1([C:18]2[CH:19]=[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:6]3[C:2]([CH3:1])=[N:3][N:4]([CH:8]4[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]4)[C:5]=3[N:7]=2)[CH2:16][CH2:17]1참가 물질
4
반응 조건
- 온도
- 70 °C
실험 절차
3-Methyl-1-(1-methyl-4-piperidinyl)-1H-pyrazol-5-amine (500 mg, 2.57 mmol) and ethyl 4-cyclopropyl-2,4-dioxobutanoate (474 mg, 2.57 mmol) were suspended in Toluene (10 mL) and heated at 70° C. for 5 h. The solvent was removed in vacuo and the crude residue was purified via silica gel chromatography (eluent: gradient of 0 to 10% MeOH:DCM). The final product was collected as a solid, 0.722 g (76%). LCMS E-S (M+H)=343.1 1H NMR (400 MHz, DMSO-d6) δ ppm 1.03-1.11 (m, 4 H), 1.38 (t, J=7.07 Hz, 3 H), 1.83 (d, J=6.06 Hz, 2 H), 2.12-2.22 (m, 4 H), 2.27 (s, 3 H), 2.35 (m, J=7.83, 7.83, 5.05, 4.80 Hz, 1 H), 2.54 (s, 3 H), 2.94 (d, J=6.57 Hz, 2 H), 4.42 (q, J=7.16 Hz, 2 H), 4.57-4.73 (m, 1 H), 7.46 (s, 1 H).