Sep-21 News A new synthetic route of 101-32-6

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 101-32-6, 2,2-(Benzylimino)diethanol.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 101-32-6, name is 2,2-(Benzylimino)diethanol. A new synthetic method of this compound is introduced below., Recommanded Product: 2,2-(Benzylimino)diethanol

2-[Benzyl-(2-hydroxyethyl)amino]ethanol (XIX); 16.9 ml (142 mmol) of benzyl bromide were added to a stirred solution of 15.0 g (142 mmol) of diethanolamine and 39.4 g (285 mmol) of potassium carbonate in 200 ml of acetone, and the solution was then heated under reflux for 3 h. The cooled reaction mixture was filtered and concentrated in vacuo. 100 ml of water were added, and the aqueous mixture was extracted with chloroform (3×60). The combined organic phases were washed with water and saturated NaCI solution and dried over magnesium sulfate, and the solvent was removed in vacuo. Yield: 26.9 g (96%) of colorless oil The reaction product was converted into the hydrochloride by dissolving the residue in 70 ml of 5N ethereal HCI and removing the solvent in vacuo. The residue was then coevaporated with toluene twice. Yield: 31.7 g (99%) of colorless oil 1H-NMR (DMSOd6): 2.51-2.59 (m, 2H), 3.41-3.48 (m, 4H), 3.65 (s, 2H), 4.34 (bs, 2H), 7.16-7.36 (m, 5H). MS (API-ES,pos) m/z = 196 [M+H]+

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 101-32-6, 2,2-(Benzylimino)diethanol.

Reference:
Patent; ABBOTT GMBH & CO. KG; WO2008/25736; (2008); A1;,
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Analyzing the synthesis route of 101-32-6

At the same time, in my other blogs, there are other synthetic methods of this type of compound,101-32-6, 2,2-(Benzylimino)diethanol, and friends who are interested can also refer to it.

Related Products of 101-32-6, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 101-32-6, name is 2,2-(Benzylimino)diethanol. A new synthetic method of this compound is introduced below.

Synthesis was performed according to the published procedure[17] with some alterations as mentioned below. 2,2′-(Benzylazanediyl)bis(ethan-1-ol) (759 mg, 3.89 mmol) in anhydrous THF (40 mL) was transferred into the two-necked flask under argon atmosphere. A solution of 1 M potassium tert-butoxide in THF(8.03 g, 71.56 mmol) was slowly injected into the reaction mixture. Pentaethylene glycol di(p-toluenesulfonate) (2.12 g, 3.89 mmol) was dissolved in anhydrous THF (20 mL) and added to the reaction mixture dropwise. The mixture was stirred for 2.5 h at 40 C. TLCanalysis (ethyl acetate/MeOH 5:1, Rf of 4 = 0.29) indicated that thereaction was completed immediately. THF was evaporated under reduced pressure. The product was dissolved in ethyl acetate (50 mL) and extracted with 5% hydrochloric acid (v/v) (3 x 50 mL).T he water layer was collected, and neutralized by 1 M NaOH and the product was extracted three times with ethyl acetate(3 x 80 mL). The organic layer was collected and evaporated todryness. The crude product was purified by column chromatographyon silica with ethyl acetate/MeOH/TEA 15:1:0.1 as an eluent. After some impurities were washed out, the mobile phase was changed to ethyl acetate/MeOH/TEA 15:3:1 as the eluent. Yield: 792 mg (51%) of colorless oil. 1H NMR (500 MHz, CDCl3, 25 C):d 2.74-2.93 (m, 4H, CH2), 3.59-3.72 (m, 26 H, CH2) and 7.22e7.41 ppm (m, 5 H, Bn-H); MS (APCI): m/z 398.7 [MH]. The other analytical data corresponded well with data published in the literature

At the same time, in my other blogs, there are other synthetic methods of this type of compound,101-32-6, 2,2-(Benzylimino)diethanol, and friends who are interested can also refer to it.

Reference:
Article; Lochman, Lukas; Svec, Jan; Roh, Jaroslav; Novakova, Veronika; Dyes and Pigments; vol. 121; (2015); p. 178 – 187;,
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