成人免费xx,国产又黄又湿又刺激不卡网站,成人性视频app菠萝网站,色天天天天

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

1032314-85-4

BenzaMide, N-[4-Methyl-3-[[4-(6-Methyl-3-pyridinyl)-2-pyriMidinyl]aMino]phenyl]-4-[(4-Methyl-1-piperazinyl)Methyl]- synthesis

4synthesis methods
Benzamide, N-[3-[(1,6-dihydro-6-oxo-2-pyrimidinyl)amino]-4-methylphenyl]-4-[(4-methyl-1-piperazinyl)methyl]-

1451042-78-6
0 suppliers
inquiry

659742-21-9 Synthesis
6-Methylpyridine-3-boronic Acid

659742-21-9
222 suppliers
$12.00/250mg

BenzaMide, N-[4-Methyl-3-[[4-(6-Methyl-3-pyridinyl)-2-pyriMidinyl]aMino]phenyl]-4-[(4-Methyl-1-piperazinyl)Methyl]-

1032314-85-4
3 suppliers
inquiry

-

Yield:1032314-85-4 51%

Reaction Conditions:

Stage #1: 4-[(4-methyl-1-piperazinyl)methyl]-N-[4-methyl-3-[(4-oxo-2-pyrimidinyl)amino]-phenyl]benzamidewith triethylamine;bromo-tris(1-pyrrolidinyl)phosphonium hexafluorophosphate in 1,4-dioxane at 45; for 1.5 h;Inert atmosphere;
Stage #2: (6-methylpyridin-3-yl)boronic acidwith bis-triphenylphosphine-palladium(II) chloride in 1,4-dioxane at 20; for 1 h;Inert atmosphere;
Stage #3: with sodium carbonate in 1,4-dioxane;water; for 24 h;Inert atmosphere;Reflux;

Steps:

6 4-[(4-Methyl-1-piperazinyl)methyl]-N-[4-methyl-3-[[4-(6-methylpyridin-3yl)-2-pyrimidinyl]amino]-phenyl]benzamide (WBZ-4)

To a suspension of 4-[(4-methyl-1 -piperazinyl)methyl]-N-[4-methyl-3-[(4- oxo-2-pyrimidinyl)amino]phenyl]benzamide (0.30 g, 0.69 mmol) in purified dioxane (15 ml) PyBrOP (0.34 g, 0.73 mmol) and triethylamine (0.29 ml, 2.1 mmol) were added under argon. The mixture was stirred at 45 °C for 1.5 h. Then 6-methyl-3-pyridylboronic acid (0.10 g, 0.73 mmol) and Pd(PPh3)2Cl2 (24.3 mg, 5 mol-%) there were added and the reaction was stirred at ambient temperature for 1 h. After aqueous Na2CO3 solution (2.1 ml, 1 mol/L; 2.1 mmol) was transferred into mixture by syringe the reaction was refluxed for 24 h under argon. Reaction mixture diluted with ethyl acetate (30 ml) and brine (5 % solution) was filtered through celite. Organic phase was separated and dried. After evaporation of solvent under reduced pressure the residue was treated with methanol to obtain 0.18 g (51 %) of title compound. Analytical sample could be obtained by flash chromatography (EtOAc:MeOH 10: 1 followed by the eluent with addition of NH4OH). M.p. 202- 205°C 1 H NMR (DMSO-ofe): 2.15 (s,3H), 2.21 (s,3H), 2.25- 2.45 (m, 8H), 2.52 (s,3H), 3.52 (s, 2H), 7.19 (d J= 8.5 Hz, 1 H) 7.37 (d J= 8.5 Hz, 1 H), 7.38 (d J= 5.2 Hz, 1 H), 7.43 (d J= 8.3 Hz, 2H), 7.48 (dd J= 8.2; 2.2 Hz, 1 H), 7.90 (d J= 8.3 Hz, 2H). 8.05 (d J= 2.0 Hz, 1 H), 8.36 (dd J= 8.2; 2.3 Hz, 1 H), 8.47 (d J=5.2 Hz, 1 H), 8.93 (s, 1 H), 9.14 (d J=2.3 Hz), 10.15 (s, 1 H).

References:

WO2013/120852,2013,A1 Location in patent:Page/Page column 15; 16