95%DISCONTINUED 10/25/01.Chemicalbook can provide 2 synthetic routes" /> angelababy床戏视频,美女视频黄的免费视频,不可说赵丽颖霍建华演唱视频

天堂网亚洲,天天操天天搞,91视频高清,菠萝蜜视频在线观看入口,美女视频性感美女视频,95丝袜美女视频国产,超高清美女视频图片

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!

ChemicalBook CAS DataBase List Panobinostat Carboxylic Acid Methyl Ester Hydrochloride
441741-66-8

Panobinostat Carboxylic Acid Methyl Ester Hydrochloride synthesis

2synthesis methods
-

Yield:441741-66-8 55%

Reaction Conditions:

with 1,8-diazabicyclo[5.4.0]undec-7-ene;lithium chloride in N,N-dimethyl-formamide at 0 - 25; for 6 h;Inert atmosphere;Reagent/catalyst;Solvent;Temperature;

Steps:

Synthesis of (E)-methyl 3-[4- ({[2- (2-methyl-1H-indol-3-yl)ethyl]amino}methyl)phenyl]acrylate hydrochloride (4)

A mixture of 2-(2-methyl-1H-indol-3-yl)ethanamine (1, 1.5 g, 9 mmol), DMF (10 mL), DBU (3.8 g, 25 mmol), LiCl (0.04g, 1 mmol) and methyl diethylphosphonoacetate (6, 5.2 g, 25 mmol) was stirred at 0 °C under a nitrogen atmosphere for 10 min, and then this mixture was slowly treated with a solution of 4-(chloromethyl)benzaldehyde (5, 1.5 g, 10 mmol) in DMF (5 mL). The reaction was then warmed to room temperature and stirred at this temperature for 6 h to give a red solution. Water (50 mL) was added to quench the reaction and it was extracted with ethyl acetate (2 × 50 mL). The combined organic layer was washed with brine and dried over anhydrous Na2SO4and filtered. Then saturated HCl/1,4-dioxane solution was added to this filtrate until pH = 2-3, and concentrated to dryness. The residue was stirred in hot ethyl acetate/EtOH for 10 min, and the resulting precipitate was filtered and dried to give the pure compound 4as: Brown solid; yield 1.8 g (55%); m.p. 239-243 °C (lit. 12245-247 °C); 1H NMR (600 MHz, DMSO-d6): δ: 2.34 (s, 3H), 2.92 (m, 2H), 3.17 (m, 2H), 3.74 (s, 3H), 4.21 (t, J= 5.8 Hz, 2H), 6.72 (d, J= 16.1 Hz, 1H), 7.01 (m, 2H), 7.25 (d, J= 8.0 Hz, 1H), 7.46 (d, J= 7.8 Hz, 1H), 7.65 (d, J= 8.2 Hz, 2H), 7.69 (d, J= 16.1 Hz, 1H), 7.80 (d, J= 8.2 Hz, 2H), 9.59 (brs, 2H), 10.90 (s, 1H); 13C NMR (150 MHz, DMSO-d6): δ11.6, 21.0, 47.4, 49.8, 52.0, 66.8, 105.6, 111.0, 117.6, 118.7, 119.0, 120.6, 128.2, 128.9, 130.9, 133.1, 134.9, 135.6, 144.2, 167.0; MS (ESI) m/z[M + H]+: 349.0; HRMS m/z calcd for C22H24O2N2[M + H]+: 349.1911; found: 349.1914.

References:

Chen, Shanwen;Zhang, Peiming;Chen, Huali;Zhang, Pu;Yu, Yu;Gan, Zongjie [Journal of Chemical Research,2018,vol. 42,# 9,p. 471 - 473]

Panobinostat Carboxylic Acid Methyl Ester Hydrochloride Related Search: