氯碳酸酯与胺反应制备脲

mg, 0.72 mmol) and diisopropylethylamine (0.46 g, 3.6 mmol) at roomtemperature. The reaction mixture was stirred at for 30 min before diluted with50 mL of CH2Cl2. The mixture was washed with 1 M NaHSO4 (3 x 50 mL), 2% Na2CO3 (3 x 50 mL) and brine (3 x50 mL). The organic phase was dried and concentrated to the crude product,which was purified by column chromatography to afford 0.61 g of [3-(6-hydroxyhexyl)ureido]aceticacid benzyl Ester (86%) as white solid..

3、 利用盐酸对甲基一锅法内甲基解释器（J. Med. Chem. 2001, 1021-1024）

To a solution of 1-(2,6-dichloro-benzyl)-3-pyrrolidin-1-ylmethyl-1H-indazol-6-ylamine(374 mg, 1.0 mmol) and diisopropylethylamine (640 mg, 5.0 mmol) in 100 mL ofDCM was added a solution of 4-nitrophenyl chloroformate (220 mg, 1.1 mmol) in10 mL of DCM at –20 oC under N2 atmosphere. The resultingmixture was stirred for 30 min and then added 3-amino-4-(3,4-difluoro-phenyl)-1-phenyl-butan-2-one(275 mg, 1.0 mmol). After stirred at – 20 oC for 30 min, the mixturewas warmed to room temperature and then stirred for another 6 h before pouredinto water. The reaction mixture was extractedwith DCM (3 x 100 mL). The combined organic phases were washed with brine (3 x50 mL), dried over anhydrous Na2SO4 and filtered. Thefiltrate was concentrated to the crude product, which was purified by columnchromatography to afford 175 mg of 1-[1-(2,6-dichloro-benzyl)-3-pyrrolidin-1-ylmethyl-1H-indazol-6-yl]-3-[1-(3,4-difluoro-benzyl)-2-oxo-3-phenyl-propyl]-urea (26 %)

4、 盐酸对甲基应用于仲衍生物的内甲基解释器（J. Med. Chem. 1999, 5254-5265）

To a solution of 5-oxo-5-piperidin-3-yl-3-pyridin-3-yl-pentanoicacid methyl ester (2.9 g, 10 mmol) in DCM (200 mL) wasadded 4-nitrophenylchloroformate (2.0 g, 10 mmol) and NMM (6.0 mL, 30 mmol) at0 oC. The resulting mixture was stirred for 2 h before poured intowater (15 mL). After separated, the organic layer was dried over anhydrous Na2SO4 and evaporatedto oil, which was dissolved in 100 mL of MeCN. The solution was then treated by[4,4']bipiperidinyl-1-carboxylic acid tert-butyl ester (4.3 g, 15 mmol) and DMAP(1.2 g, 10 mmol), and heated to reflux for 24 h. After removal of the solvent,the residue was dissolved in EtOAc (200 mL). The organic phase was washed with 1N NaOH (3 x 100 mL), brine (3 x 100 mL) and dried over anhydrous Na2SO4. Afterfiltered, the filtrate was concentrated to the crude product, which was purifiedby silica gel chromatography to afford 4.1g of 1'-[3-(4-methoxycarbonyl-3-pyridin-3-yl-butyryl)-piperidine-1-carbonyl]-[4,4']bipiperidinyl-1-carboxylicacid tert-butyl ester (69 %)

本文内容来源于网络服务，授权归制作者所有。

。

肩颈痛怎么治疗效果好
兰州治白癜风哪家医院好
艾得辛和来氟米特有什么区别
艾得辛治疗类风湿效果怎么样
骨关节炎吃什么药可以止痛