Isoquinoline sulfonyl derivatives and their applications
A drug and compound technology, applied in the field of isoquinolinesulfonyl derivatives and their pharmaceutical compositions, can solve the problems of unsatisfactory pharmacokinetic properties and hERG activity, and achieve low potential risk, reduced clearance rate, and improved half-life Effect
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Embodiment 1
[0072]
[0073] first step
[0074] A solution of 1a (30.00g, 173.24mmol), triethylamine (43.83g, 433.00mmol) in N,N dimethylformamide (500mL) was cooled to 0°C and O-(7-azabenzotriazepine was added Azol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphine salt (79.05 g, 208.00 mmol). The resulting reaction solution was stirred at 0°C for 10 minutes. Then N-methoxymethylamine hydrochloride (18.59 g, 191.00 mmol) was added and stirred at 20° C. for 16 hours. The reaction solution was poured into water (1.00L) and extracted with ethyl acetate (2.00L x2). The combined organic phases were dried over anhydrous sodium sulfate, filtered and evaporated to dryness. The crude product was separated and purified on a silica gel column (petroleum ether / ethyl acetate = 100-0%), yielding 1b.
[0075] 1 H NMR (400MHz, CD 3 OD) δ4.13-4.07(m, 2H), 3.74(s, 3H), 3.37(s, 1H), 3.21(s, 3H), 1.37-1.35(m, 2H), 1.26-1.22(m, 3H) ), 1.03-1.00 (m, 2H).
[0076] second step
[0077] To a solut...
Embodiment 2
[0097]
[0098] first step
[0099] Compound 1h and compound 2a were synthesized according to compound 1 to obtain compound 2.
[0100] MS-ESI calculated value [M+H] + 364, the measured value is 364.
[0101] 1 H NMR (400MHz, D 2 O) δ9.30(s, 1H), 8.67(s, 1H), 8.62(d, J=7.6Hz, 1H), 8.46(d, J=8.4Hz, 1H), 7.86(t, J=8.0Hz , 1H), 4.05-3.94(m, 2H), 3.82-3.77(m, 1H), 3.57-3.55(m, 1H), 3.38-3.22(m, 2H), 2.42-2.39(m, 1H), 2.08 -2.04 (m, 1H), 1.06-0.79 (m, 4H).
Embodiment 3
[0103]
[0104] first step
[0105] Compound 1h and compound 3a were synthesized according to compound 1 to obtain compound 3.
[0106] MS-ESI calculated value [M+H] + 348, the measured value is 348.
[0107] 1 H NMR (400MHz, CD 3 OD) δ9.25(s, 1H), 8.67(d, J=8.0Hz1H), 8.53(d, J=8.0Hz, 1H), 8.45(d, J=8.0Hz, 1H), 7.86(t, J =8.0Hz, 1H), 3.85-3.73(m, 2H), 3.43(s, 1H), 3.06-2.98(m, 1H), 2.72-2.65(m, 1H), 2.15-2.05(m, 1H), 1.73-1.71 (m, 1H), 0.97-0.87 (m, 1H), 0.82-0.79 (m, 2H), 0.69-0.60 (m, 2H).
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