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氯化钴/邻菲罗啉催化氯苄双羰化合成苯丙酮酸的研究 总被引:2,自引:0,他引:2
双羰化是制备α-酮酸及其衍生物的重要反应 ,因其反应途径简捷且收率高而倍受青睐 ,国内外有不少关于氯苄双羰化合成苯丙酮酸的报道 .1 982年发现的钯配合物主要用于催化芳基卤代物的双羰化 [1] ;金子林等[2 ] 进行了八羰基二钴催化氯苄双羰化合成苯丙酮酸的研究 ,李光兴等[3 ] 近期也报道了吡啶 - 2 -羧酸钴的催化氯苄高效合成苯丙酮酸 .受前期吡啶 - 2 -羧酸钴催化双羰化研究成果的启发 ,我们进一步探讨了不同的席夫碱与氯化钴组成的催化体系的双羰化性能 .实验发现 ,采用“一锅煮”的方式 ,将氯化钴和邻菲罗啉 ( Phen)按一定比例加入到… 相似文献
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Frank曾报道了苯乙酮三重态敏化α-蒎烯价键异构化的工作.本文以9,10-二氰基蒽(DCA)为敏化剂,重点研究了苯溶液中α-蒎烯的异构化反应,确定反应产物为荣烯和顺式罗勒烯;同时对反应机制进行了简要的讨论. 实验仪器 Finnigan Model 4021 C型气相色谱-质谱联用仪.Shimadzu GC-7AG气相色谱仪.Hitachi MPF-4型荧光光谱仪.Hitachi 340型紫外-可见分光光谱仪. 试剂α-蒎烯为上海试剂一厂产品.气相色谱确定其纯度为97%,含3%β-蒎烯;DCA系伊思曼柯达公司产品;荣烯由黄岩桔子油提取,b.p.176℃,其IR、MS均与标准谱完全一致;顺式罗勒烯按文献[1]制备. 相似文献
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Hosomi等人曾报道了1-α-氯代-2,3,4,6-四-O-苄基-D-吡喃葡萄糖(1)与烯丙基硅醚反应主要得到α异构体占优势的烯丙基碳苷。我们研究了化合物1在Lewis酸存在下和芳香醚反应,结果发现,产物都是β构型的芳香碳苷。这与Schmidt等人和Williams等 相似文献
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采用气相色谱法跟踪测定了α-蒎烯氧化反应中主产物蒎酮酸的含量;实验结果表明,在SE-30/Chro-mosorb W/AW(0.25-0.175mm)的色谱柱上,蒎酮酸与副产物之间具有较好的分离效果,并且在峰形对称性和出峰时间上,SE-30柱也具有优势;该法操作简便、快速、准确性高、重复性好;对同一试样的5次平行独立测定的相对标准偏差(RSD)为1.8%;该法的标准加入回收率达88%-96%。 相似文献
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F. M. Avotin'sh M. V. Petrova N. N. Tonkikh A. Strakov 《Chemistry of Heterocyclic Compounds》2000,36(11):1326-1328
Beckmann rearrangement of N-[3-(1-hydroxyimino)ethyl-2,2-dimethylcyclobutyl]acetylanthranilic acid, and its 5-bromo and 4-chloro derivatives gives the corresponding N-(3-acetylamino-2,2-dimethylcyclobutyl)acetylanthranilic acids. Treatment of these acylanthranilic acids with formamide gives 2-(3-acetylamino-2,2-dimethylcyclobutyl)methyl-4(3H)-quinazoline and its 6-bromo and 7-chloro derivatives. 相似文献
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Zapevalov A. Ya. Filyakova T. I. Kodess M. I. Saloutin V. I. 《Russian Journal of Organic Chemistry》2003,39(7):919-923
Epoxidation of 3-chloro(bromo)heptafluoro-1-butenes and 3,4-dichlorohexafluoro-1-butene with aqueous solutions of sodium hypohalites is accompanied by cleavage of the carbon skeleton at the double bond and formation of polyfluorocarboxylic acid sodium salts as by-products. 3-Chloro(bromo)-1,2-epoxy- heptafluoro- and 3,4-dichloro-1,2-epoxyhexafluorobutanes were synthesized and subjected to isomerization into carbonyl compounds by the action of cesium fluoride or antimony pentafluoride. 相似文献
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G. V. Bozhenkov V. A. Savosik L. I. Larina L. V. Klyba E. R. Zhanchipova A. N. Mirskova G. G. Levkovskaya 《Russian Journal of Organic Chemistry》2008,44(7):1014-1023
2-Chlorovinyl alkyl ketones react with alkylhydrazines to give mixtures of 1-R-3-R′- and 1-R-5-R′-pyrazoles: The 1-R-3-R′-pyrazoles form through the heterocyclization of 2-chlorovinyl ketone alkylhydrazones whereas in the heterocyclization into 1-R-5-R′-pyrazoles N 1-alkyl-N 2-(2-acylvinyl)hydrazines are involved. The regiospecific heterocyclization of 2-chloro-and 2,2-dichlorovinyl ketones with arylhydrazines and also of 2,2-dichloro(bromo)vinyl trifluoromethyl ketones with C alkylhydrazines into pyrazoles and 5-chloro(bromo)-pyrazoles proceeds through a stage of haloenones hydrazones formation. The study of the structure of the obtained 1-alkyl-3(5)-alkylpyrazoles by means of two-dimenaional 1H and 13C NMR spectroscopy and GC-MS method made it possible to assign the proton and carbon signals of isomeric pyrazoles and to establish the diagnostic ions for the pair of 1,3-and 1,5-isomers. 相似文献
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L. I. Khusainova L. O. Khafizova T. V. Tyumkina U. M. Dzhemilev 《Russian Journal of Organic Chemistry》2014,50(3):309-313
A selective procedure has been developed for the synthesis of 1-chloro(bromo)-substituted borolanes and 2,3-dihydro-1H-boroles by reaction of aluminacarbocycles with boron trihalides BX3 (X = Cl, Br). 3-Substituted 1-chloro(bromo)borolanes and 2,3-dihydro-1H-boroles have been isolated as individual substances, and their structure has been determined. 相似文献
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F. M. Avotin'sh M. V. Petrova P. V. Pastors A. Ya. Strakov 《Chemistry of Heterocyclic Compounds》1999,35(6):722-728
Anthranilic acid and its 5-bromo and 4-chloro derivatives react with pinanoic and pinonoic acid chlorides to give the corresponding N-acyl derivatives. The pinanoyl derivatives give the corresponding 2-(3-ethyl-2,2-dimethyl-cyclobutylmethyl)-4-(3H)-quinazolinones when refluxed in formamide. Pinanoylanthranilic acid reacts with dicyclohexylcarbodiimide to give 2-(3-ethyl-2,2-dimethylcyclobutylmethyl)benz-3,1-oxazin-4(H)-one and subsequently with hydrazine hydrate to give 3-amino-2-(3-ethyl-2,2-dimethylcyclobutylmethyl)-4(3H)-quinazolinone. Refluxing of the pinanoyl- and pinonoylanthranilic acids with acetic anhydride gives acetylanthranilic acid, and pinonoylanthranilic acid gives 4(3H)-quinazolinone with formamide.Riga Technical University, Riga LV-1658, Latvia; e-mail: marina@osi.lanet.lv. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 811–817, June, 1999. 相似文献
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In the nitration of 3-(4-nitrophenyl)-1-phenyl-2,2-dichloroaziridine in acetic acid, 1-(o- and p-nitrophenyl)-derivatives are formed in a 35:65 ratio. 1,3-Di-phenyl-2,2-dichloroaziridine undergoes opening of the three-membered ring under the same conditions, forming a mixture of o- and p-nitroanilides and 2-nitro-4-chloroanilides of 2-acetoxy (or 2-chloro)-2-phenylacetic acids. The bromination of 3-(4-nitrophenyl)-1-phenyl-2,2-dichloroaziridine in aqueous acetic acid leads to 1-(4-bromophenyl)-3-(4-nitrophenyl)-2,2-dichloroaziridine, while in a mixture of acetic acid and acetic anhydride it leads to the anilide of 2-bromo-2-phenyl-acetic acid and 2-bromo-N-(2,4-dibromophenyl)-1-(4-nitrophenyl)-2,2-dichloro-ethylamine.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 7, pp. 912–916, July, 1984. 相似文献
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N. S. Prostakov E. V. Kruglyak V. P. Shalimov N. D. Sergeeva 《Chemistry of Heterocyclic Compounds》1990,26(1):63-65
4-Aza-fluoren-9-ol and 9-chloro(bromo)-4-azafluorenes are converted in high yields upon refluxing with thionyl chloride to form bis[9-chloro(bromo)-4-azafluoren-9-yl]. At about 20C, azafluorenol and thionyl chloride form 9-chloro-4-azafluorene. Mechanisms are proposed for these reactions.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 72–74, January, 1990. 相似文献
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Ya. R. Tymyanskii S. M. Aldoshin M. I. Knyazhanskii O. A. D'yachenko A. I. Pyshchev L. O. Atovmyan 《Russian Chemical Bulletin》1982,31(3):478-482
Conclusions It was found by UV spectroscopy and x-ray diffraction analysis that the photocyclization of 1-(3'-halophenyl)-2,4,6-triphenylpyridiniurn cations leads to stable 1,3-diphenyl-11-chloro(bromo)-azoniatriphenylene cations.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 3, pp. 535–540, March, 1982. 相似文献
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Treatment of 9-(2,3,5-tri-O-acetyl-beta-d-ribofuranosyl)-2-amino-6-chloropurine (1) with TMS-Cl and benzyltriethylammonium nitrite (BTEA-NO2) in dichloromethane gave the crystalline 2,6-dichloropurine nucleoside 2, and acetyl chloride/BTEA-NO2 was equally effective ( approximately 85%, without chromatography). TMS-Br/tert-butyl nitrite/dibromomethane gave crystalline 2-bromo-6-chloro analogue 3 (85%). (Chloro or bromo)-dediazoniation of 3',5'-di-O-acetyl-2'-deoxyadenosine (4) gave the 6-[chloro (5, 63%) or bromo (6, 80%)]purine deoxynucleosides, and 2',3',5'-tri-O-acetyladenosine (8) was converted into the 6-chloropurine nucleoside 9 (71%). 相似文献
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N. A. Nedolya N. P. Papsheva A. V. Afonin V. A. Kukhareva T. V. Kashik B. A. Trofimov 《Russian Chemical Bulletin》1993,42(2):310-314
Reactions of 2-vinyloxyethyl isothiocyanate with aliphatic halocarboxylic acids give rise to their 1-(2-isothiocyanatoethoxy)ethyl esters in quantitative yields. An unusual rearrangement of 1-(2-isothiocyanatoethoxy)ethyl chloro(bromo)acetate and 3-bromopropanoate to 5-aza-7-chloro(bromo)-4-oxo-3-thiaheptanoic and to 6-aza-8-bromo-5-oxo-4-thiaoctanoic acids, respectively, was observed. Monohalocarboxylic acids and their esters were shown to readily alkylate l,3-oxazolidine-2-thione to form the same thiaheptanoic and thiaoctanoic acids and their esters.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 350–354, February, 1993. 相似文献