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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol. A new synthetic method of this compound is introduced below., name: 4-(Dimethylamino)butan-1-ol
General procedure: 12 (100 mg, 0.35 mmol) was dissolved in the mixture of 1,4-dioxane (10 mL) and H2O (2.00 mL) and then added with boronicacid (2.80 mmol), Pd(dppf)2Cl2 (28 mg, 0.035 mmol) and Cs2CO3(228 mg, 0.70 mmol). The reaction was heated at 100 C underargon atmosphere. After 12 h, the reaction mixture was cooled toroom temperature and was concentrated in vacuo. Then themixture was diluted with water and extracted with ethyl acetate.The combined organic layer was washed by saturated sodiumchloride solution for three times, dried over anhydrous Na2SO4 andconcentrated under reduced pressure. The residue was purified bysilica gel chromatography to give 13.To a stirred solution of 13 and triphosgene (100 mg, 0.34 mmol)in anhydrous dichloromethane (5 mL) was added triethylamine(104 mg, 1.02 mmol) at 0 C under nitrogen atmosphere. After5 min, a solution of 4-(dimethylamino)butan-1-ol (1.02 mmol) indichloromethane (5.00 mL) was added and then the mixture wasstirred at room temperature for overnight. The reactionwas dilutedwith dichloromethane (15 mL) and washed with water (3 20 mL).The organic phases were dried over anhydrous Na2SO4 andconcentrated in vacuo. The residue was purified by using columnchromatography to afford the corresponding product.
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Reference:
Article; Lu, Dong; Liu, Jianan; Zhang, Yunzhe; Liu, Feifei; Zeng, Limin; Peng, Runze; Yang, Li; Ying, Huazhou; Tang, Wei; Chen, Wuhong; Zuo, Jianping; Tong, Xiankun; Liu, Tao; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 328 – 337;,
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