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With potassium tert-butylate;palladium diacetate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene; In 1,4-dioxane; at 100℃; for 18h;
Example 16. f4-(4-MethvI-piperazine-l-suIfonvI)-phenvIl-(5-nitro-pyrimidin-2-yl)- amine (11); [0146] 5-Nitro-pyrimidin-2-ylamine (1.78 mmol, 1.0 equiv), l-(4-bromo- benzenesulfonyl)-4-methyl-piperazine (2.68 mmol, 1.5 equiv), Pd(OAc)2 (0.089mmol, 0.05eq), Xantphos (0.178 mmol, 0.1 equiv) and potassium-t-butoxide (3.56 mmol, 2.0 equiv) were suspended in 15 mL of dioxane and refluxed at 100C under an argon atmosphere for 18 h. The mixture was allowed to cool to room temperature, filtered and washed with DCM. The filtrate was concentrated under reduced pressure and a silica plug was run to purify material (5% MeOH/DCM) to afford the title compound as a pale yellow solid (758 mg, 95%). MS (ES+): m/z = 379 (M+H)+. LC retention time: 1.76 min.
With potassium tert-butylate;palladium diacetate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene; In 1,4-dioxane; for 15h;Heating / reflux;
Example 128. 2-{4-f2-MethvI-6-(5-nitro-pyrimidin-2-ylaminoVpyrimidm-4-yll- piperazin-l-yl}-etlianol (72); [0308] A mixture of 5-nitro-pyrimidin-2-ylamine (0.45 g, 3.2 mmol), compound 71 described in Example 127 (1.0 g, 3.9 mmol), Pd(OAc)2 (50 mg, 0.22 mmol), Xantphos (0.26 g, 0.45 mmol) and potassium tert-butoxide (0.72 g, 6.4 mmol) were suspended in dioxane (15 niL) and heated at reflux under the argon atmosphere for 15 h. The mixture was allowed to cool to room temperature, filtered and washed with DCM. The filtered solid was washed with water and DCM to afford the title compound (0.60 g, 52%), which was used in the next step without further purification. MS (ES+): m/z 361 (M+H)+.
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