Pharmaceutical compounds
A technology of compounds and oxides, applied in drug combination, organic chemistry, antineoplastic drugs, etc., can solve problems such as arrhythmia
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Embodiment 1 to 4
[0878] The compounds of Examples 1 to 4 were prepared as described above.
[0879]
[0880]
Embodiment 5
[0882] 5A. tert-butyl 4-tert-butoxycarbonylamino-4-(4-chloro-benzylcarbamoyl)-piperidine-1-carboxylate
[0883]
[0884] Anhydrous DMF (1 mL) was added to a mixture of mono-tert-butyl 4-tert-butoxycarbonylamino-piperidine-1,4-dicarboxylate (151 mg, 0.44 mmol) and HATU (220 mg, 0.58 mmol) under nitrogen. mixture. N-Ethyldiisopropylamine (0.38 mL, 2.1 mmol) was added to the solution, and the reaction mixture was stirred for 15 minutes. 4-Chlorobenzylamine (70 uL, 0.57 mmol) was added and the solution was stirred at room temperature under nitrogen for 23 hours. The reaction mixture was partitioned between dichloromethane (10 mL) and water (10 mL). The aqueous phase was further extracted with dichloromethane (20 mL). The combined organic layers were dried (Mg 2 SO 4 ), filtered and concentrated. Elution with 4% methanol in dichloromethane and flash column chromatography on silica afforded 4-tert-butoxycarbonylamino-4-(4-chloro-benzylcarbamoyl)-piperidine-1 - tert-butyl f...
Embodiment 6
[0895] 1-thieno[3,2-d]pyrimidin-4-yl-piperidin-4-yl-amine
[0896] 6A. (1-Thieno[3,2-d]pyrimidin-4-yl-piperidin-4-yl)-tert-butyl carbamate
[0897]
[0898] The title compound (AT11980) was prepared using the method of Example 5, except piperidin-4-yl-carbamic acid tert-butyl ester was used in place of 4-amino-piperidine-4-carboxylic acid 4-chloro-benzylamide.
[0899] LC / MS: (LCT1)[M+H] + 334,R t 4.62min
[0900] 6B.1-Thieno[3,2-d]pyrimidin-4-yl-piperidin-4-yl-amine
[0901]
[0902] A solution of the product from Example 6A in 2M HCl (2ml) was stirred at room temperature for 2 hours and then evaporated to dryness. Solid-phase extraction on SCX-II acidic resin (elution with MeOH followed by 1M NH in MeOH 3 elution) to obtain the deprotected product. LC / MS (LCT1): [M+H] + 234,R t 0.85min. 1 H(250MHz, MeOD) δ8.45(1H, s), 8.04(1H, d, J=5.5Hz), 7.38(1H, d, J=5.5Hz), 4.95-4.81(2H, m), 3.34- 3.29(2H,m), 3.08-2.98(1H,m), 2.06-2.00(2H,m), 1.52-1.36(2H,m).
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