O-glycoprotein-2-acetamido-2-deoxy-3-d-glycopyranosidase inhibitors
A CR2R2, C3-C10 technology, applied in the field of O-glycoprotein-2-acetylamino-2-deoxy-3-D-pyranosidase inhibitors, can solve problems such as complex application
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Embodiment 1-1
[0163]
[0164] N-(5-((3-(4-fluorobenzyl)piperidin-1-yl)methyl)thiazol-2-yl)acetamide: to 3-(4-fluorobenzyl)piperidine (0.054g , 0.279 mmol) in MeOH (15.0 mL) were added N-(5-formylthiazol-2-yl)acetamide (0.095 g, 0.559 mmol) and a drop of AcOH. The mixture was stirred at 50 °C for 2 h. Add NaBH 3 CN (0.053 g, 0.838 mmol) and the mixture was stirred at 50 °C for 17 h. By preparative HPLC {(column: Waters Xbridge PrepOBD C18 150x30 5u; condition: water (0.04%NH 3 h 2 O+10mM NH 4 HCO 3 )-MeCN; Start at B: 35; End at B: 65; Gradient time (min): 10; 100% B hold time (min): 2; Flow rate (ml / min): 25} Purify the mixture to provide the title compound (0.038g, 39%). LCMS: [M+H] 348. 1 HNMR: (400MHz, methanol-d4) δ7.19(s, 1H), 7.14-7.10(m, 2H), 6.94(t, J=9.2Hz, 2H), 3.65(s, 2H), 2.83-2.75( m,2H),2.48(d,J=6.8Hz,2H),2.19(s,3H),2.02-1.99(m,1H),1.82-1.66(m,4H),1.57-1.47(m,1H) ,0.99-0.91(m,1H).
Embodiment 1-2
[0166]
[0167] N-(5-((3-(pyridin-2-ylmethyl)piperidin-1-yl)methyl)thiazol-2-yl)acetamide: to 2-(3-piperidinylmethyl)pyridine To a suspension of HCl (0.035 g, 0.165 mol, hydrochloride) and N-[5-(chloromethyl)thiazol-2-yl]acetamide (0.032 g, 0.165 mmol) in MeCN (0.64 mL) was added Triethylamine (0.05 g, 0.494 mol) and the mixture was warmed to 70 °C overnight. The reaction was cooled to room temperature, and the mixture was diluted with EtOAc and washed with saturated NH 4 Cl(aq) washes. via MgSO 4 The organics were dried, filtered and concentrated in vacuo. The residue was purified by preparative HPLC {(column: Waters XSelect CSH PrepC18 5um OBD 19x100mm; conditions: water: MeCN gradient 5-55% ACN, 7min gradient, 0.1 Vol% aluminum hydroxide modifier} to afford the title compound (0.015 g, 27%). LCMS (ESI): [M+H] 331. 1 HNMR: (500MHz, CDCl 3 )δ11.76(br s,1H),8.45(dd,J=1.8,4.9Hz,1H),8.40(d,J=1.8Hz,1H),7.47(td,J=1.8,7.9Hz,1H) ,7.21(dd,J=4.6,7.0Hz,1H),7.18(s,1H),3.70-3.5...
Embodiment 1-3
[0169]
[0170] N-(5-((3-(3-methoxybenzyl)piperidin-1-yl)methyl)thiazol-2-yl)acetamide: The title compound was obtained from 3- ((4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)methylene)piperidine-1-carboxylic acid tert-butyl ester, 1-bromo-3 - Preparation from methoxybenzene and N-(5-formylthiazol-2-yl)acetamide. LCMS (ESI): [M+H] 360. 1 HNMR: (400MHz, methanol-d4) δ7.20(s, 1H), 7.13(t, J=8.0Hz, 1H), 6.71-6.69(m, 3H), 3.75(s, 3H), 3.71-3.65( m,2H),2.84-2.78(m,2H),2.48-2.46(m,2H),2.19(s,3H),2.04-1.99(m,1H),1.88-1.66(m,4H),1.58- 1.48(m,1H),1.00-0.92(m,1H).
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