Showing papers on "Boron tribromide published in 2012"
TL;DR: The protocol makes functionalizations of aryl CH bonds easy and uses cheap and readily available boron tribromide as the borylating reagent, and inorganic salts as the functional group sources.
Abstract: Selective functionalizations of aryl CH bonds in 2-arylpyridines have been developed via sequential borylation and aerobic oxidative copper catalysis, and the corresponding aryl halides, sulfones, azides and arylamines were obtained in good yields. The protocol uses cheap and readily available boron tribromide (BBr3) as the borylating reagent, and inorganic salts (potassium iodide, ammonium bromide, sodium alkylsulfinates, sodium azide) as the functional group sources. This method makes functionalizations of aryl CH bonds easy.
39 citations
Patent•
20 Jun 2012
TL;DR: In this paper, a 1-(1-substituted benzyl-5-methyl)-1H-1,2,3-triazole-4-yl)-3-substantituted benyl-3-hydroxy-2-propylene-1-ketone compound and a preparation method and an application thereof were discussed.
Abstract: The invention relates to (Z)-1-(1-substituted benzyl-5-methyl-1H-1,2,3-triazole-4-yl)-3-substituted benzyl-3-hydroxy-2-propylene-1-ketone compound and a preparation method and an application thereof. The compound is expressed by formula (I), wherein R1 represents -F, R2 represents -H, or R1 represents -H, R2 represents -F; R3, R4 and R5 represent -OH or -H. The preparation method of the compound comprises synthesizing fluoro-benzyl azide with mono-fluoro benzyl bromide as raw material, reacting with acetylacetone to obtain 1-(1-fluoro-benzyl)-4-acetyl-5-methyl)-1H-1,2,3-triazole, carrying out condensation reaction with substituted methyl benzoate to obtain a compound having a dicarboxylic acid structure, and finally demethylating with boron tribromide to obtain the compound. The compound provided by the invention has an inhibitory action to HIV-1 (human immunodeficiency virus-1) integrase.
3 citations
Patent•
28 Mar 2012
TL;DR: The triptolide is a main active compound from the separation of the tripterygium root as discussed by the authors, and is a key intermediate in the prior triptoline synthesis method.
Abstract: The invention provides a method for preparing a triptolide intermediate with the following formula, belonging to the chemical synthesis filed. The tripterygium root is a traditional Chinese medicinal material. The triptolide is a main active compound from the separation of the tripterygium root. The inventive method takes 5-methoxyl-2-tetralone and 2-(2-iodine ethyl)-1, 4-butyrolactone as initial materials and obtains the intermediate through coupling reaction under the action of N-p-Trifluromethyl benzyl chiral quaternary ammonium bromide and the sodium hydroxide, aminolysis reaction of lactonic ring, hydroxyl oxidation into aldehyde group, intramolecular aldol condensation, etherification reaction of enol silyl of the aldehyde group, selective hydrogenation reduction reaction, oxidation of benzyl methylene into carbonyl, breakage of methyl ether bond under the action of boron tribromide, and friedel-crafts isopropyl reaction. The intermediate is a key intermediate in the prior triptolide synthesis method.
2 citations
Patent•
11 Jul 2012
TL;DR: In this paper, a bis(pinacolato)diboron production process is described in which boron trichloride is used as a raw material and is aminated with dimethylamine gas in an n-hexane system, the desalinated reaction solution and borón tribromide react at the room temperature, the prepared intermediate and magnesium are coupled in toluene, 1, 2-dichloroethane solution of pinacol is dropped into the desalinized reaction solution, and the target product is prepared via
Abstract: The invention discloses a bis(pinacolato)diboron production process which is characterized in that boron trichloride is used as a raw material and is aminated with dimethylamine gas in an n-hexane system, the desalinated reaction solution and boron tribromide react at the room temperature, the prepared intermediate and magnesium are coupled in toluene, 1, 2-dichloroethane solution of pinacol is dropped into the desalinated reaction solution, and the target product is prepared via transesterification The invention has the advantages that: n-hexane is used as a reaction solvent for the first two steps, the conversion rate of reaction is increased, and the ultra low temperature can be avoided; the safety of the process is improved due to use of magnesium; and the yield of the product is increased in transesterification through controlling the reaction temperature
2 citations
Patent•
07 Nov 2012
TL;DR: In this article, an aryne-based boron polymer is presented, which is structurally characterized by containing bboron atoms and arynes-based groups, and a three-step reaction under the protection of inert gas is performed.
Abstract: The invention discloses an aryne-based boron polymer and a preparation method thereof. The aryne-base boron polymer is structurally characterized by containing boron atoms and aryne-based groups. The preparation method of the aryne-based boron polymer comprises the following steps: taking diacetylene-benzene, phenylacetylene, boron chloride or boron tribromide, organic metallic compounds and pyridine as raw materials, synthesizing the aryne-based boron polymer by three-step reaction under the protection of inert gas; and firstly, adopting the organic metallic compounds to prepare the aryne-based metallic compound, then carrying out complexing on boron chloride or boron tribromide and pyridine to form complex, and then carrying out polymerization on the aryne-based metallic compound and the boron chloride complex to obtain the aryne-based boron polymer. The invention has the advantages of simple technique, convenient operation, short reaction time, easy control of technique conditions and simple process of aftertreatment. The aryne-based boron polymer synthesized by the invention is red brown sticky liquid, or faint yellow solid or faint yellow crystal, is stable under the normal temperature, is easy to store, and can form a cross-linked curing structure by light and heat polymerization.
2 citations
Patent•
25 Jul 2012
TL;DR: In this article, an oxime ether isomerization method was described, which takes Lewis acid as a catalyst, Z-typed isomer oxime isomer 2-alcoxyl imino group replaces methyl phenyl acetate in an aprotic solvent to be converted into E-ttyped oxime methyl acetate, wherein, the R1 substituting group is halogen, nitro group, cyanogen group, C1-C4 alkyl groups, C 1 -C4 halogenated groups, phenyl group and substituting phen
Abstract: The invention discloses an oxime ether isomerization method The method takes Lewis acid as a catalyst, Z-typed isomer oxime ether 2-alcoxyl imino group replaces methyl phenyl acetate in an aprotic solvent to be converted into E-typed oxime ether; wherein, the R1 substituting group is halogen, nitro group, cyanogen group, C1-C4 alkyl groups, C1-C4 halogenated alkyl groups, phenyl group and substituting phenoxy methyl group or substituting phenoxy; the R2 substituting group is C1-C4 alkyl groups The Lewis acid contains titanium tetrachloride, aluminum trichloride and boron tribromide The isomerization method has the advantages of simple operation, easy control and no pollution
1 citations
Patent•
10 Oct 2012
TL;DR: In this paper, a preparation method of Baculiferin l and analogs thereof is presented, which is characterized by fewer steps, simple process, and high yield; and precious metal catalysts are not needed.
Abstract: The invention discloses a preparation methodof Baculiferin L and analogs (see the following formula) thereof I is prepared under protection of inert gas by a substituted phenylacetaldehyde and an amino compound or ammonia gas; II is obtained through a reaction between I and 2-bromo-2-(3,4-dimethoxy benzyl) acetic acid trichloroethyl alcohol ester under an condition of acidic alumina; III is obtained through a reaction among II and zinc dust and an ammonium acetate solution; IV is obtained through a reaction among III and potassium acetate and acetic anhydride; V is obtained through a reaction in an organic solvent between IV and a sodium hydroxide solution; Baculiferin L and analogs thereof are obtained under protection of inert gas by V and boron tribromide in the presence of organic solvent The method is characterized by fewer steps, simple process, and high yield; and precious metal catalysts are not needed The method saves energy, reduces emission, and has high efficiency The invention also discloses the anti-AIDS related applications of Baculiferin L and analogs thereof aiming at AIDS key targets like Vif, APOBEC3G, pg41, and the like
1 citations
Patent•
11 Jan 2012
TL;DR: In this article, a bis(pinacolato)diboron production process is described in which boron trichloride is used as a raw material and is aminated with dimethylamine gas in an n-hexane system, the desalinated reaction solution and borón tribromide react at the room temperature, the prepared intermediate and magnesium are coupled in toluene, 1, 2-dichloroethane solution of pinacol is dropped into the desalinized reaction solution, and the target product is prepared via
Abstract: The invention discloses a bis(pinacolato)diboron production process which is characterized in that boron trichloride is used as a raw material and is aminated with dimethylamine gas in an n-hexane system, the desalinated reaction solution and boron tribromide react at the room temperature, the prepared intermediate and magnesium are coupled in toluene, 1, 2-dichloroethane solution of pinacol is dropped into the desalinated reaction solution, and the target product is prepared via transesterification. The invention has the advantages that: n-hexane is used as a reaction solvent for the first two steps, the conversion rate of reaction is increased, and the ultra low temperature can be avoided; the safety of the process is improved due to use of magnesium; and the yield of the product is increased in transesterification through controlling the reaction temperature.
Patent•
19 Jul 2012
TL;DR: In this paper, a paraterphenyl derivative has been described, which has a compound structural formula shown as formula (I), wherein R1 = hydroxyl or methoxyl; R2 = hydrogen, hydroxy or methoxide; R3 = hydrogen or methoxyoxycycline; R4 = hydrogen and hyroxycycline.
Abstract: Disclosed is a paraterphenyl derivative, which has a compound structural formula shown as formula (I), wherein R1 = hydroxyl or methoxyl; R2 = hydrogen, hydroxyl or methoxyl; R3 = hydrogen, hydroxyl or methoxyl; R4 = hydrogen, hydroxyl or methoxyl; R5 = hydroxyl or methoxyl; and R6 = hydroxyl or methoxyl. The compound in this invention is obtained by Suzuki coupling and demethylating of boron tribromide. A test shows that the paraterphenyl derivative described in this invention has higher cytotoxin activity and potential of being developed into antitumor medicaments.
Patent•
21 Nov 2012
TL;DR: In this paper, a synthetic method for triassic boron nitride synthesis is described, where trimethyl azide silane is added to a reactor at 15-30 DEG C, followed by an organic solvent containing Boron tribromide under agitation.
Abstract: The invention discloses a synthetic method of triassic boron nitride. The method comprises the steps of: adding trimethyl azide silane into a reactor at 15-30 DEG C; adding an organic solvent containing boron tribromide under agitation; reacting for 2-9 hours at 0-70 DEG C after the organic solvent containing boron tribromide is added; distilling reaction liquid at normal pressure; collecting fraction at 42-45 DEG C; and obtaining triassic boron nitride, wherein the molar ratio of boron tribromide to triassic boron nitride is 1 to 3-4, and the organic solvent is ethyl acetate, trichloromethane or acetonitrile. The synthetic method is mainly applied to synthesis of triassic boron nitride.