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CAS No. : | 5961-59-1 | MDL No. : | MFCD00008399 |
Formula : | C8H11NO | Boiling Point : | - |
Linear Structure Formula : | (CH3)NH(C6H4)(OCH3) | InChI Key : | JFXDIXYFXDOZIT-UHFFFAOYSA-N |
M.W : | 137.18 | Pubchem ID : | 22250 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P264-P270-P272-P280-P301+P312+P330-P302+P352-P305+P351+P338-P333+P313-P337+P313-P501 | UN#: | N/A |
Hazard Statements: | H302-H317-H320 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With sodium acetate; In tetrahydrofuran; water; at 60 - 70℃; for 3h; | A mixture of <strong>[105763-77-7]2,4-dichloro-6-methoxy-quinazoline</strong> (0.5 g, 2.18 mmol), (4-methoxy-phenyl)-methyl-amine (0.35 g, 2.61 mmol) and sodium acetate (0.21 g, 2.61 mmol) in 8 mL of solvent (1:1 THF:water) was stirred at 60-70 C. for 3 h. The reaction mixture was concentrated and the resulting solid was dissolved in ethyl acetate and filtered through a pad of silica, washing with 40% ethyl acetate/hexane. The filtrate was concentrated under reduced pressure to give 0.7 g of the title compound (98% yield). 1H NMR (DMSO-d6) delta 7.6 (d, 1H), 7.36-7.31 (m, 3H), 7.08-7.05 (dd, 2H), 6.2 (d, 1H), 3.79 (s, 3H), 3.5 (s, 3H), 3.28 (s, 3H); LC-MS (ESI+; 330 ([M+H]+). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
0.58 g | With N-ethyl-N,N-diisopropylamine; HATU; In N,N-dimethyl-formamide; at 20℃; | HATU (0.800 g, 2.10 mmol) was added to a stirred solution of 4-methoxy-N- methylaniline (0.240 g, 1.75 mmol), (S)-2-((tert-butoxycarbonyl)amino)-3 -(3- hydroxyphenyl)propanoic acid (0.493 g, 1.75 mmol) and DIPEA (0.92 mL, 5.3 mmol) in DMF (5 mL) and the reaction mixture was stirred at RT overnight. The reaction was diluted with water (50 mL), extracted with EtOAc (2 X 40 mL) and thecombined organic component was concentrated to dryness and purified (40g 5i02, 0-30% EtOAc/DCM) to yield the title compound (0.58 g). LC-MS retention time =1.99 mm; mlz = 399.3 [M-Hf. (Column: Phenonenex-Luna C18 2.0 x 30mm 3 pm.Solvent A = 95% Water:5% Acetonitrile: 10 pM ammonium acetate. Solvent B =5% Water:95% Acetonitrile: 10 pM ammonium acetate. Flow Rate = 1.0 mL/min.Start % B = 0. Final % B = 100. Gradient Time = 3 mm. Wavelength = 220). ?HNMR (400MHz, CHLOROFORM-d) oe 7.10 (t, J=7.8 Hz, 1H), 6.91 - 6.66 (m, 5H),6.52 (d, J=7.6 Hz, 1H), 6.46 (s, 1H), 5.57 (br. s., 1H), 5.20 (d, J=7.6 Hz, 1H), 4.52 (d,J=7.8 Hz, 1H), 3.81 (s, 3H), 3.19 (s, 3H), 2.84 (dd, J=13.0, 7.8 Hz, 1H), 2.68 (dd,J=12.8, 6.2 Hz, 1H), 1.40 (br. s., 9H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97.6% | With tris-(dibenzylideneacetone)dipalladium(0); potassium carbonate; (R)-2,2'-bis(diphenylphosphanyl)-1,1'-binaphthyl; In acetonitrile; at 25℃; for 3.5h;Inert atmosphere; | General procedure: 6-Chloro-5-nitropyrimidine-4-amine (0.5mmol), amine (1.5mmol), Pd2(dba)3 (0.01mmol), R-BINAP (0.03mmol) and potassium carbonate (0.7mmol) were dissolved in acetonitrile (5mL). The solution was stirred at room temperature for 3.5h under an argon atmosphere. The resulting reaction mixture was treated with saturated brines (50mL) and extracted with acetonitrile (3×25mL), and dried with anhydrous Na2SO4. The anhydrous Na2SO4 was removed by filtration and the filtrate was concentrated. The residue was washed with ethyl acetate (3×2mL) and diethyl ether (3×2mL), filtered and dried under vacuum. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | With palladium diacetate; caesium carbonate; 2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl; In toluene; at 100℃; for 12h;Inert atmosphere; | To a stirred solution of 4-methoxy-N-methylaniline ([5961-59-1], 3.6 g, 26.27 mmol) and <strong>[18442-22-3]7-bromochroman-4-one</strong> ([18442-22-3], 7.15 g, 31.53 mmol) in toluene (40 mL) were added Cs2C03 (17.07 g, 52.54 mmol), BINAP (1.31 g, 2.10 mmol) and Pd(OAc)2 (0.47 g, 2.10 mmol). The reaction was stirred at 100 C for 12 h under inert atmosphere. The mixture was partitioned between water and EtOAc. The organic layer was concentrated and purified by silica-gel column chromatography [gradient elution with 10% EtOAc in Hexane] to afford the target compound (2.9 g, 40.0%) as a brown solid. LCMS MH+ calculated, 284.1, found, 284.2. |
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