Novel pyrrole derivatives
A drug and compound technology, applied in the field of new pyrrole derivatives, can solve disadvantages and other problems
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[0100] Acronym
[0101] AcOH glacial acetic acid
[0102] aq.
[0103] Bn benzyl
[0104] Br wide
[0105] Boc tert-butoxycarbonyl
[0106] COPD chronic obstructive pulmonary disease
[0107] d doublet
[0108] DCM dichloromethane
[0109] DIPEAN, N-Diisopropylethylamine
[0110] DMAP4-dimethylaminopyridine
[0111] DMFN, N-Dimethylformamide
[0112] DMSO Dimethyl Sulfoxide
[0113] EDC1-ethyl-3-(3-dimethylaminopropyl)carbodiimide
[0114] EtOAc ethyl acetate
[0115] h hours (or hours)
[0116] HATUN,N,N′,N′-tetramethyl-O-(7-azobenzotriazol-1-yl)urea PF6
[0117] HPLC High Performance Liquid Chromatography
[0118] m multiplet
[0119] MeCN acetonitrile
[0120] MeOH Methanol
[0121] min minutes (or minutes)
[0122] NMR nuclear magnetic resonance
[0123] PBS Phosphate Buffered Saline
[0124] quin. quintet
[0125] RT room temperature
[0126] s unimodal
[0127] sat. Saturated
[0128] SAX solid supported strong cation exchange resin
[0129] sept. ...
Embodiment A1
[0149] Example A1: 3,4-Dihydroxy-1-(4-methoxyphenyl)-N 2 ,N 2 ,N 5 ,N 5 -Tetramethyl-1H-pyrrole-2,5-dicarboxamide (UL1-005)
[0150]
[0151] Step (i): Diethyl 2,2'-((4-methoxyphenyl)azanediyl)diacetate (1)
[0152] Ethyl 2-bromoacetate (146 mL, 1.30 mol) was added dropwise to a stirred solution of 4-methoxyaniline (75.0 g, 0.610 mol) and DIPEA (265 mL, 1.50 mol) in MeCN (300 mL). The reaction mixture was stirred at 60 °C for 16 h, then partitioned in 2M HCl (水溶液) (500 mL) and EtOAc (300 mL), the aqueous phase was extracted with EtOAc (300 mL), and the combined organics were sequentially extracted with 2M HCl (水溶液) (2×300mL), water (500mL) and brine (500mL), dried (MgSO 4 ), filtered and the solvent was removed in vacuo to give diethyl 2,2'-((4-methoxyphenyl)azanediyl)diacetate (1) (180 g, 100%) purple oil: m / z296(M+H) + (ES + ). 1 HNMR (400MHz, CDCl 3 )δ6.82-6.78(m,2H),6.64-6.59(m,2H),4.19(q,J=7.1Hz,4H),4.10(s,4H),3.74(s,3H),1.27(t , J=7.1Hz, 6H).
[0153] St...
Embodiment A2
[0163] Example A2: 3,4-dihydroxy-1-(4-methoxyphenyl)-N 2 ,N 2 ,N 5 ,N 5 - Alternative potential synthesis of tetramethyl-1H-pyrrole-2,5-dicarboxamide (UL1-005)
[0164]
PUM
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