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乙酰化氧

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We investigated constituent of triterpenoid saponins ofAlbizzia, two new compounds together with two known compounds were isolated from Albizzia julibrissin Durazz. by using column chromatography (macroreticular resin, silica gel, Sephadex gel, reverse phase silica gel),preparative HPLC methods et al.On the basis of spectroscopic analysis, including IR,ESI-MS,~1H-NMR,~(13)C-NMR,HMBC,HMQC,~1H-~1HCOSY and chemical methods, the structure of two new compounds were identified as 3 - O -[β-D-xylopyranosyl(1→2)-β-D-fucopyranosyl (1→6)-β- D -2- deoxy - 2 - acetoamidoglucopyranosyl] -21-O-[(6S)-2- trans- 2,6-dimethyl - 6 - O-β- D - quinovopyranosyl -2,7- octadienoyl] - acacic acid- 28 - O-β-D-glucopyranosyl(1→3)[α-L-arabinofuranosyl(1→4)]-α-L-rhamnopyranosyl(1→2)-β-D-glucopyranoside acacic acid 3- O -β- D- glucopyranosy(1→3)-β- D- fucopyranosl(1→6) [β-D- xylopyranosyl (1→2)]-β-D-glucopyranoside ;two known compounds were acacic acid lactone 3- O -β-D- xylopyranosyl-(1→2)-β-D-fucopyranosl (1→6)- 2-deoxy -2 -acetoamido -β-D- glucopyranoside ; acacic acid lactone 3- O-β-D-xylopyranosyl(1→2)-α-L- arabinopyranosl (1→6)- 2- deoxy - 2- acetoamido -β-D-glucopyranoside . The study lays chemical foundation and chemical reference substance for enhancing quality standard of Albizzia julibrissin Durazz.

本研究论文在综述国内外对合欢属Albizzia三萜皂苷化学成分和药理作用研究进展的基础上,利用传统植化分离手段和现代分离技术,包括大孔树脂、硅胶、葡聚糖凝胶、反相硅胶等柱色谱,制备高效液相色谱法等技术从中药合欢皮中分离得到了4个化合物,其中,2个新化合物和2个己知化合物,并进一步通过现代分析技术IR,ESI-MS,~1H-NMR,~(13C-NMR,HMBC,HMQC,~1H-~1HCOSY等和化学方法鉴定了2个新化合物的结构分别是:3-O-[β-D-吡喃木糖基(1→2)-β-D-吡喃夫糖基(1→6)-β-D-2-去氧-2-乙酰氨基吡喃葡萄糖基]-21-O-[(6S)-2-反式-2,6-二甲基-6-O-β-D-吡喃鸡纳糖基-2,7-辛二烯酸基]-金合欢酸-28-O-α-L-呋喃阿拉伯糖基(1→4)[β-D-吡喃葡萄糖基(1→3)]-α-L-吡喃鼠李糖基(1→2)-β-D-吡喃葡萄糖苷,金合欢酸3-O-β-D-吡喃葡萄糖基(1→3)-β-D-吡喃夫糖基(1→6)[β-D-吡喃木糖基(1→2)]-β-D-吡喃葡萄糖苷;2个已知化合物结构分别是:金和欢酸内酯3-O-β-D-吡喃木糖基(1→2)-β-D-吡喃夫糖基(1→6)-β-D-2-去氧-2-乙酰氨基吡喃葡萄糖苷,金和欢酸内酯3-O-β-D-吡喃木糖基(1→2)-α-L-吡喃阿拉伯糖基(1→6)-β-D-2-去氧-2-乙酰氨基吡喃葡萄糖苷。

In this thesis, a convenient and efficient synthesis of highly functionalizeddihydropyrido[2,3-d]pyrimidines via a double [5 + 1] annulation strategy startingfrom easily available α-alkenoyl-α-carbamoyl ketene--acetals 1 and cheapreagents (NH4OAc, DMF, and POCl3) has been developed.

本论文探索了一种简便有效的合成高度官能化的二氢吡啶并[2,3-d]嘧啶的方法,此方法由易得的α-乙酰基-α-氨基乙酰基二硫缩烯酮1和便宜的试剂(醋酸铵,二甲基甲酰胺和三氯氧磷)通过两步[5 + 1]加成而实现。

In a system consisting of 20% PEG 400 and 12% magnesium sulfate, the partition coefficient of PGA was less than 0.01, PGA almost completely partitioned into the magnesium sulfate-rich bottom phase. Meanwhile, the partition coefficient of cephalexin was 6.7, the partition coefficients of phenylglycine methyl ester and 7-ADCA were 1.5 and 1.2, respectively.

通过考察头孢氨苄、苯甘氨酸甲酯和7-氨基脱乙酰氧基头孢烷酸(7-ADCA)在ATPS中的分配行为建立了一个含20%PEG 400和12%硫酸镁的ATPS,在此体系中头孢氨苄的分配系数为6.7,苯甘氨酸甲酯的分配系数为1.5,7-ADCA的分配系数为1.2,且青霉素酰化酶的分配系数小於0.01。

Results show that, by using thionyl chloride and N,N-dimethyl formamide as chlorinating reagent and dichloromethane as solvent and taking -15℃ as reaction temperature, Z-iomer crystals with pale white color and stable to temperature can be obtained with an overall yield of 70%.

以2-(2-氨基噻唑-4-基)-2-甲氧亚氨基乙酸为原料,经盐酸化、氯代等反应合成了Z-2-(2-氨基噻唑-4-基)-2-甲氧亚氨基乙酰氯盐酸盐;氯代时以用亚硫酰氯和N,N-二甲基甲酰胺的混合物代替五氯化磷作氯化剂,并考察了温度和溶剂对氯代产物中Z-异构体和E-异构体收率的影响。

Formyl-3-acetyl-4-methyl-5-carbobenzoxypyrrole (6) was synthesized via the selective oxidation of 2,4-dimethyl-3-acetyl-5-carbobenzoxypyrrole (5), which was produced from acetylacetic benzylester (1) via nitrosation, reduction and addition-cyclization with acetylacetone. The total yield of the product was about 34%.

以乙酰乙酸苄酯(1)为原料,经过亚硝化、还原、与乙酰丙酮加成环化生成2, 4-二甲基-3-乙酰基-5-苄氧羰基吡咯(5),通过选择性氧化反应制得目标化合物2-甲酰基-3-乙酰基-4-甲基-5-苄氧羰基吡咯(6),反应的总收率约为34%。

Spiral Spirobifluorene acetylated is oxidated by m-chloroperoxybenzoic acid and hydrolyzed by sodium hydroxide ,obtaining 2,2 '- dihydroxy -9,9'- spiral Spirobifluorene .Through nitrification,Reduced by hydrazine hydrate, we may get the 2,2 '- diamino -9,9'- spiral Spirobifluorene which are characterizated by IR, 1H-NMR !

L-酒石酸和乙醇酯化得到酒石酸二乙酯,将保护羧基保护起来,然后用碘甲烷在2,3-位上两个甲基,得到2,3-二甲氧基-酒石酸二乙酯,再用氢氧化钠将其水解,得到2,3-二甲氧基-酒石酸,用五氯化磷将羧基酰化,得到2,3-二甲氧基- 1,4-丁二酰氯,经过与二环己胺反应,得到拆分配体2,3-二甲氧基–N,N,N',N'-四环己丁二酰胺。

A process for preparingp-fluo-2-(2-methyl-3-propionyl)-4-oxy-N,3-diphenyl-phenylbutylamide includes such steps as Friedle-Craft acylating of newly prepared phenylacetyl chloride and fluorobenzene under catalysis of AlCl3 to obtain 4-fluoro-phenylbenzyl ketone, brominating at carbonyl alpha position under catalysis of less AlCl3 to obtain alpha-bromo-4-fluo-phenylbenzyl ketone, and condensing with isobutyryl acetanilide under action of sodium ethoxide.

本发明涉及一种制备对氟-2-(2-甲基-3-氧丙基)-4-氧-N,3-二苯基-苯丁酰胺(1)的方法,其包括以下步骤:新制的苯乙酰氯与氟苯在AlCl3催化下进行Friedle-Craft酰化反应,得到对4-氟-苯基苄基酮(4);化合物(4)在少量AlCl3催化下进行羰基α位溴化,得到α-溴-4-氟-苯基苄基酮(5);然后(3)异丁酰乙酰苯胺在乙醇钠作用下与化合物(5)进行缩合。

The α-monobromination of 2-pentone,4-methyl acetophenone,4-methoxyacetophenone,6-methoxy-2-acetylnaphthane,2,2,5,5-tetramethyl-3-hexanone,cyclooctanone,cyclododecanone with respectively,were studied.

研究了离子液体三溴化1-丁基-3-甲基咪唑[Br3]对2-戊酮、4-甲基苯乙酮、4-甲氧基苯乙酮、6-甲氧基-2-乙酰基萘、2,2,5,5-4-甲基-3-己酮、环辛酮、环十二酮、丁醛等羰基化合物的α-溴化反应。

NOBS PAG , can obviously activate hydrogen peroxide thus , the efficiency of hydrogen peroxide bleaching can be advanced greatly .

研究结果初步表明,此类有机酰化剂类如:四乙酰乙二胺,四乙酰甘脲,异壬酰氧基苯磺酸钠,五乙酰葡萄糖等有着非常明显的活化过氧化氢的作用,从而能在很大程度上提高纸浆过氧化氢漂白的效率。

Following resolution, the following steps are performed: reduce the isomer to an alcohol, react the alcohol with triphenylmethyl chloride, ozonalyze the resulting reaction product, reduce the ozonalyzed product to yield a diol and react the diol with a methane sulfonyl compound to form-3-2-{(methylsulfonyloxy}ethoxy-4--1-butanol methane sulfonate.

拆分后,进行下一步:将异构体还原为醇,使醇与三苯基甲基氯反应,臭氧化所得反应产物,还原臭氧化产物以得到一种二醇并使所述二醇与甲烷磺酰基化合物反应以形成-3-2-{(甲基磺酰基氧}乙氧基-4--1-丁醇甲烷磺酸酯。

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