一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
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 5-Fluoro-2-methylaniline
367-29-3

5-Fluoro-2-methylaniline synthesis

6synthesis methods
In a nitrogen-fed glovebox, Pd(P(o-tol)3)2 and CyPF-PtBu (1:1 ratio) were dissolved in dioxane and mixed for 5 min. A 20 mL scintation vial was charged with aryl halide (0.60 mmol, 1 equiv), ammonium sulfate (0.90 mmol, 1.5 equiv), and sodium tert-butoxide (2.7 mmol, 4.5 equiv). To this vial was added 6 mL of anhydrous dioxane and the appropriate amount of catalyst from the stock solution. The reaction vial was sealed with a Teflon-lined screw cap and removed from the glovebox. The reaction was stirred at the desired temperature for 12 h. The reaction mixture was diluted with EtOAc and filtered through a pad of Celite. The filtrate was concentrated in vacuo, and the crude product was purified by flash column chromatography. 5-Fluoro-2-methylaniline (Table 3, 2s) (CAS: 367-29-3) The reaction to form this product was conducted with 0.5 mol % Pd(P(o-tol)3)2 and 0.5 mol % CyPF-PtBu for 8 h. The crude product was isolated by flash column chromatography (5:1 Hexanes:EtOAc). 5-Fluoro-2-methylaniline was isolated as an oil in 76% yield. 1(600 MHz, CDCl3): δ 6.97 (t, J= 7.2 Hz, 1H), 6.40 (t, J= 9.9 Hz, 2H), 3.69 (s, 2H), 2.12 (s, 3H). 13C-NMR(151 MHz, CDCl3): δ 162.24 (d, JC-F= 240.9 Hz), 145.82 (d, JC-F= 10.6 Hz), 131.12 (d, JC-F= 9.6 Hz), 117.62 (d, JC-F = 2.6 Hz), 104.67 (d, JC-F= 21.0 Hz), 101.56 (d, JC-F= 24.6 Hz), 16.62 (s).
5-Fluoro-2-methylaniline synthesis
-

Yield:367-29-3 70%

Reaction Conditions:

with hydrogenchloride;iron in ethanol;water at 0; for 12 h;Reflux;

Steps:

1.1 Step-i: Synthesis of 5-fluoro-2-methylaniline
4-Fluoro-1-methyl-2-nitrobenzene (2.50 g, 16 mmol) was dissolved in ethanol (50 mL).To this solution, iron powder (4.50 g, 81 mmol) and 0.25 ml of HC1 were added at 0 °C and the reaction mixture was refluxed for 12h. After completion of reaction, reaction mixture was cooled to room temperature, diluted with ethyl acetate, filtered through Celite and washed with ethyl acetate. Filtrate was basified with sodium bicarbonate solution; organic layer was washed with water followed by brine solution. Organic layer was dried over anhydrous Na2SO4 andconcentrated under reduced pressure to obtain crude compound. The residue was purified by column chromatography (n-hexane/ EtOAc 1:1) to give the title compound (1.4 g, 70 %) as a light brown solid.‘H NMR (400 MHz, DMSO-d6): ? 6.87 (t, J = 7.6 Hz, 1H), 6.38-6.34 (m, 1H), 6.22-6.18 (m, 1H), 5.11 (bs, 2H), 1.99 (s, 3H). MS (ES) mle: 126 (M+1).

References:

AURIGENE DISCOVERY TECHNOLOGIES LIMITED;GUMMADI, Venkateshwar Rao;SAMAJDAR, Susanta;GUPTA, Ajay WO2015/104662, 2015, A1 Location in patent:Page/Page column 37

FullText

5-Fluoro-2-methylaniline Related Search:

离岛区| 宽甸| 通江县| 麻栗坡县| 揭东县| 利津县| 湘西| 余江县| 壶关县| 内乡县| 河北区| 鱼台县| 渭源县| 林口县| 德保县| 秀山| 抚松县| 濮阳市| 崇州市| 丰原市| 兰溪市| 错那县| 塘沽区| 嘉义县| 阿坝| 焉耆| 滕州市| 扶沟县| 婺源县| 公安县| 枣阳市| 江阴市| 林口县| 循化| 绵竹市| 林州市| 上饶县| 绍兴市| 阿尔山市| 东光县| 阜新|