7, 9-nitrogen radical-4-oxo-4h-pyrido[l,2-a]pyrimidine-2-carboxylic acid benzylamide anti-virals
An alkyl and aryl technology, applied in the field of new bicyclic pyrimidinone (pyrimidinone) compounds, can solve problems such as drug resistance
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Embodiment 1
[0210] Example 1: N-(4-fluorobenzyl)-3-hydroxyl-7-(4-methylpiperazin-1-yl)-4-oxo-9-(2-oxo-1,3- Preparation of oxazin (oxazinan)-3-yl)-4H-pyrido[1,2-a]pyrimidine-2-carboxamide
[0211]
[0212] [1,3]oxazinyl-2-ones were prepared according to the literature Journal of Heterocyclic Chemistry, 1966, 3(1), 84-89 using the starting materials (raw materials) described in Synthesis Scheme 1 .
Embodiment 11
[0213] Example 1.1: Methyl-3-(benzyloxy)-7-bromo-4-oxo-9-(2-oxo-1,3-oxazin-3-yl)-4H-pyrido[1 ,2-a] the preparation of pyrimidine-2-carboxylate
[0214]
[0215] [1,3]oxazinyl-2-one (235 mg, 2.23 mmol), 3-(benzyloxy)-7-bromo-9-iodo-4-oxo-4H-pyrido[1,2- a] methyl pyrimidine-2-carboxylate (1 g, 1.94 mmol), Pd 2 dba 3 (179mg, 0.19mmol), 4,5-bisdiphenylphosphine-9,9-dimethylxanthene (xantphos) (224mg, 0.39mmol) and Cs 2 CO 3 (950mg, 2.9mmol) mixture in dioxane (10ml). in N 2 The mixture was heated at 90° C. for 6 hours under atmosphere. After cooling to room temperature, the dioxane was removed in vacuo. The residue was purified by column chromatography (EA / PE=1 / 1) to yield the desired product (350 mg, 40%).
[0216] 1 H NMR (300M Hz, CDCl 3 )δ9.08(d,J=2.1Hz,1H),7.79(d,J=2.1Hz,1H),7.55-7.45(m,2H),7.44–7.31(m,3H),5.34(s,2H ), 4.53(t, J=5.1Hz, 2H), 3.91(s, 3H), 3.84-3.64(m, 2H), 2.34-2.19(m, 2H).
[0217] MS (ESI + ) m / z488 (M[Br 79 ]+1),490(M[Br 81 ]+1)
Embodiment 12
[0218] Example 1.2: Methyl-3-(benzyloxy)-7-(4-methylpiperazin-1-yl)-4-oxo-9-(2-oxo-1,3-oxazine- Preparation of 3-yl)-4H-pyrido[1,2-a]pyrimidine-2-carboxylate
[0219]
[0220] The product from Example 1.1 (300 mg, 0.61 mmol), 1-methylpiperazine (123 mg, 1.23 mmol), Pd 2 dba 3 (56mg, 0.06mmol), 4,5-bisdiphenylphosphine-9,9-dimethylxanthene (69mg, 0.12mmol) and Cs 2 CO 3 (298mg, 0.92mmol) were mixed in dioxane (3ml). in N 2 The mixture was heated at 85° C. for 6 hours under atmosphere. After cooling to room temperature, the dioxane was removed in vacuo. The residue was purified by column chromatography (DCM / MeOH=20 / 1) to give the desired product (120 mg, 33%).
[0221] 1 H NMR (300M Hz, CDCl 3 )δ9.08(d,J=2.1Hz,1H),7.79(d,J=2.1Hz,1H),7.59-7.49(m,2H),7.44-7.31(m,3H),5.30(s,2H ),4.53(t,J=4.8Hz,2H),3.89(s,3H),3.84-3.70(m,2H),3.36-3.20(m,4H),2.67-2.51(m,4H),2.38( s,3H), 2.34-2.18(m,2H).
[0222] MS (ESI + )m / z508(M+1)
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