Carbamate compounds and methods of making and using same
A technology of compounds and formate esters, applied in the field of carbamate compounds and their preparation and use, can solve the problems of lack of selectivity of MAGL regulatory compounds
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Embodiment 1
[0274] Example 1: 2,5-dioxopyrrolidin-1-yl 4-(bis(benzo[d][1,3]dioxol-5-yl)(hydroxy)methyl)piper pyridine-1-carboxylate
[0275]
[0276] From bis(benzo[d][1,3]dioxol-5-yl)(piperidin-4-yl)methanol (27 mg, 0.075 mmol), DSC (19 mg, 0.075 mmol) and NMM ( 0.025 mL, 0.23 mmol) Follow Procedure A to synthesize the title compound. Purification of the crude product by flash chromatography (6:3:1 EtOAc:Hexane:MeOH) afforded the title compound (31 mg, 84%) as a white solid: 1 HNMR (400MHz, CDCl 3 )δ6.92(s,2H),6.90(d,J=8.30Hz,2H),6.74(d,J=8.34Hz,2H),5.92(s,4H),4.27–4.09(m,2H), 3.02(t,J=12.13Hz,1H),2.89(t,J=12.29Hz,1H),2.80(s,4H),2.44(t,J=11.60Hz,1H),2.19(s,1H), 1.66–1.56(m,2H),1.56–1.36(m,2H); 13 C NMR (101MHz, CDCl 3 )δ170.25, 150.65, 148.13, 146.66, 139.94, 119.15, 108.26, 107.06, 101.45, 79.62, 46.06, 45.24, 44.40, 26.65, 26.40, 25.86; for C 25 h 24 N 2 o 9 [M+Na] + Calculated HRMS (ESI-TOF+) m / z: 519.1374, found 519.1384.
Embodiment 2
[0277] Example 2: 2,5-dioxopyrrolidin-1-yl 4-[bis(4-chlorophenyl)methyl]piperazine-1-carboxylate
[0278]
[0279] The title compound was synthesized following Procedure A from 1-(bis(4-chlorophenyl)methyl)piperazine (160 mg, 0.5 mmol), DSC (130 mg, 0.50 mmol) and NMM (0.16 mL, 1.5 mmol). Purification of the crude product by flash chromatography (50% EtOAc / hexanes) afforded the title compound (180 mg, 78%) as a colorless oil: 1 H NMR (500MHz, CDCl 3 )δ7.33–7.29(m,4H),7.28–7.25(m,4H),4.24(s,1H),3.63(bs,2H),3.51(bs,2H),2.79(s,4H),2.42 (d,J=4.8Hz,3H); 13 C NMR (126MHz, CDCl 3 )δ170.14, 150.70, 140.44, 133.60, 129.42, 74.76, 51.45, 51.38, 45.54, 45.04, 25.89; for C 22 h 21 Cl 2 N 3 o 4 [M+H] + Calculated HRMS (ESI-TOF+) m / z: 462.0987, found 462.0979.
Embodiment 3
[0280] Example 3: 2,5-dioxopyrrolidin-1-yl 4-[bis(4-bromophenyl)methyl]piperazine-1-carboxylate
[0281]
[0282] The title compound was synthesized following Procedure A from 1-(bis(4-bromophenyl)methyl)piperazine (45 mg, 0.11 mmol), DSC (28 mg, 0.11 mmol) and NMM (0.036 mL, 0.33 mmol). The crude product was purified by flash chromatography (50% EtOAc / hexanes) to afford the title compound (50 mg, 83%) as an off-white crystalline solid: 1 H NMR (600MHz, CDCl 3 )δ7.42(d,J=8.32Hz,4H),7.25(d,J=8.30Hz,4H),4.21(s,1H),3.64(bs,2H),3.52(bs,2H),2.81( s,4H),2.44(bs,4H); 13 C NMR (151MHz, CDCl 3 )δ169.71, 150.26, 140.45, 131.98, 129.32, 121.32, 74.50, 51.04, 50.97, 45.11, 44.60, 25.46; for C 22 h 21 Br 2 N 3 o 4 [M+H] + Calculated HRMS (ESI-TOF+) m / z: 549.9977, found 549.9963.
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