34 results about "Diisobutylaluminium hydride" patented technology

Trace amount levels of heavy metals such as mercury in crude oil are reduced by contacting the crude oil with a sufficient amount of a reducing agent to convert at least a portion of the non-volatile mercury into a volatile form of mercury, which can be subsequently removed by any of stripping, scrubbing, adsorption, and combinations thereof. In one embodiment, at least 50% of the mercury is removed. In another embodiment, the removal rate is at least 99%. In one embodiment, the reducing agent is selected from sulfur compounds containing at least one sulfur atom having an oxidation state less than +6; ferrous compounds; stannous compounds; oxalates; cuprous compounds; organic acids which decompose to form CO2 and / or H2 upon heating; hydroxylamine compounds; hydrazine compounds; sodium borohydride; diisobutylaluminium hydride; thiourea; transition metal halides; and mixtures thereof.

Trace amount levels of heavy metals such as mercury in crude oil are reduced by contacting the crude oil with a sufficient amount of a reducing agent to convert at least a portion of the non-volatile mercury into a volatile form of mercury, which can be subsequently removed by any of stripping, scrubbing, adsorption, and combinations thereof. In one embodiment, at least 50% of the mercury is removed. In another embodiment, the removal rate is at least 99%. In one embodiment, the reducing agent is selected from sulfur compounds containing at least one sulfur atom having an oxidation state less than +6; ferrous compounds; stannous compounds; oxalates; cuprous compounds; organic acids which decompose to form CO2 and / or H2 upon heating; hydroxylamine compounds; hydrazine compounds; sodium borohydride; diisobutylaluminium hydride; thiourea; transition metal halides; and mixtures thereof.

The invention relates to a novel method for synthetizing prostaglandin analogues, and an important intermediate compound related to the novel method. The method comprises the steps of (a), just protecting 15-site hydroxyl of the compound of a formula 2 by utilizing a hydroxyl protection group under an alkaline condition; (b) restoring a lactone ketone group from DIBAL (diisobutylaluminium hydride) to obtain the intermediate of a formula 4; (c) carrying out Wittig reaction on the intermediate of the formula 4 by utilizing 4-carboxy butyl-triphenylphosphine bromide, carrying out esterification or amidation after connecting an alpha chain; (d) removing 15-site hydroxyl protection group to obtain the prostaglandin analogue of the formula 1. The method is less in side reaction, easy to monitor, and convenient to separate due to the fact that the difference between a crude product and the polarity of a process material is large.

The invention discloses a novel method for preparing a lubiprostone midbody as shown in the formula 7. The method comprises the following steps: (1), a compound as shown in the formula 1 reacts with tert-butyldimethylsilyl chloride to selectively protect a primary hydroxyl group, thereby obtaining a compound shown in the formula 2; (2), a protecting group is applied to the compound 2 under the action of a catalyst, thereby obtaining a compound shown in the formula 3; (3), after the compound 3 is reduced through diisobutylaluminium hydride, a Wittig reaction is carried out on the compound 3, thereby obtaining carboxylic acid shown in the formula 4; (4), the compound 4 is protected in an acetonitrile solvent through a protecting group, thereby obtaining a compound shown in the formula 5; (5), the compound 5 is treated by using the tert-Butyldimethylsilane for removing the protecting group, thereby obtaining a compound shown in the formula 6; and (6), the compound 6 is oxidized by an oxidant and then reacts with a compound shown in the formula (10), thereby obtaining the higher-purity compound shown in the formula 7.

The invention discloses a synthetic method of strigolactone (+ / -)-GR24 and 4-substituted (+ / -)-GR24. The method comprises the following steps: benzoic acid which is used as a raw material reacts with dibromomethane to obtain an intermediate as shown in the formula I; the intermediate I undergoes diisobutylaluminium hydride reduction to obtain an intermediate as shown in the formula II; the intermediate II and (2-carboxyethyl)triphenylphosphonium bromide undergo coupling under the action of alkali so as to obtain an intermediate as shown in the formula III; the intermediate III reacts with Dess-Martin periodinane to obtain an intermediate as shown in the formula IV; the intermediate IV undergoes cyclization under the action of an acid catalyst or reacts with a nucleophilic reagent so as to obtain ABC tricyclic lactone, namely an intermediate as shown in the formula V; the intermediate V and ethyl formate undergo a formylation reaction to obtain an intermediate VI; and the intermediate VI and bromobutenolide undergo coupling so as to obtain (+ / -)-GR24 and 4-substituted (+ / -)-GR24. The raw materials used in the synthetic method are cheap and easily available; the operation is simple; reaction conditions are mild; safety is high; the catalyst used in the invention is environment-friendly; tricyclic lactone can be constructed by one-step tandem cyclizaiton reaction; the reaction route is short; and overall yield is high. Thus, total cost is greatly reduced. The synthetic method meets requirements of mass synthesis.

The invention discloses a method for synthesizing di-tert-butylphenylphosphonium tetrafluoroborate, and belongs to the field of organic synthesis. The method comprises the following steps: in the anhydrous and anaerobic atmospheres, taking dichlorophenylphosphine as a raw material, after the reduction of diisobutyl aluminium hydride, reacting with tertiary butanol under the catalytic action of boron trifluoride, and then carrying out hydrolysis to generate the di-tert-butylphenylphosphonium tetrafluoroborate. Compared with the prior art, the method is high in yield and simple in aftertreatment, and is more applicable for industrial production.

The present invention relates to a novel method for asymmetrically synthesizing natural product (-)-Euscapholide isomers. Starting with (R)‑3‑hydroxybutyrate methyl ester, after p-methoxybenzyl protection, diisobutylaluminum hydride reduction, Mukaiyama aldol reaction, sodium borohydride reduction, acidic ring closure, hydroxyl Elimination, deprotection and other processes complete the asymmetric total synthesis of the target molecule 1. The synthetic route design is novel and reasonable, the raw materials are cheap and easy to obtain, the operation process is simple, the reaction conditions are mild, and the asymmetric total synthesis of one isomer of Euscapholide with two chiral centers is efficiently completed, and the product configuration is single.

The invention discloses a method for asymmetrically catalyzing and synthesizing (R)-4, 7-dimethyl-1-tetralone. According to the method, an asymmetrical Kumada cross coupling reaction is conducted on racemization 2-halogenated propionate ester catalyzed by bis oxazoline / cobalt and a methyl phenyl grignard reagent, and (S)-P-toluene propionate ester 2 is firstly generated; then, (S)-P-toluene propionate ester 2 is reduced to (S)-P-toluene propyl alcohol 3 through diisobutylaluminium hydride (DIBAL-H), and then (R)-4-p-methylphenyl-1-amylene 5 is obtained through bromine generation and coupling with and vinyl grignard reagent; next, a hydroboration-oxidation reaction and a Dess-Martin oxidizing reaction are sequentially conducted, and (R)-4-p-methylphenyl valeraldehyde 6 is obtained; finally, oxidation is conducted through silver oxide, an intramolecular Fourier acyl reaction is conducted, and (R)-4,7-dimethyl-1-tetralone is obtained in a ring-closure synthesis mode. The synthesis route is simple and concise, 8 reactions are conducted in all, the total yield is 27%, and the optical purity of a product is 90%.

The invention discloses a novel method for preparing a lubiprostone midbody as shown in the formula 7. The method comprises the following steps: (1), a compound as shown in the formula 1 reacts with tert-butyldimethylsilyl chloride to selectively protect a primary hydroxyl group, thereby obtaining a compound shown in the formula 2; (2), a protecting group is applied to the compound 2 under the action of a catalyst, thereby obtaining a compound shown in the formula 3; (3), after the compound 3 is reduced through diisobutylaluminium hydride, a Wittig reaction is carried out on the compound 3, thereby obtaining carboxylic acid shown in the formula 4; (4), the compound 4 is protected in an acetonitrile solvent through a protecting group, thereby obtaining a compound shown in the formula 5; (5), the compound 5 is treated by using the tert-Butyldimethylsilane for removing the protecting group, thereby obtaining a compound shown in the formula 6; and (6), the compound 6 is oxidized by an oxidant and then reacts with a compound shown in the formula (10), thereby obtaining the higher-purity compound shown in the formula 7.

The invention belongs to the technical field of organic photosensitive drums, and provides a preparation method and application of an NPB-like hole transport functional material. The NPB-like hole transport functional material comprises BTBF-DPA. The BTBF-DPA is used for an electronegative organic photoconductor drum of a laser printer. The preparation method comprises the following steps: T01, brominating benzothiophene with NBS to obtain a product A; T02, oxidizing the obtained product A with hydrogen peroxide to obtain a product B; T03, subjecting the obtained product A to a coupling reaction to obtain a product C; T04, subjecting the obtained product C to a diisobutylaluminium hydride reduction reaction to obtain a product D; T05, subjecting the obtained product D to an NBS bromination reaction to obtain a product E; T06: carrying out a ring closing reaction on the obtained product E to obtain a product F; T07, brominating the obtained product F through liquid bromine to obtain a product raw material; and T08: carrying out a Suzuki coupling reaction on the obtained product raw material to obtain the final product BTBF-DPA. The preparation method has the advantages of strict hierarchy, no need for sequential coating of a photosensitive drum structure, simple technical process, lower cost and high practical value.

The invention discloses an anti-trypanosome anticancer natural product Cryptofolione synthesizing method. The synthesizing method disclosed by the invention comprises the steps: after acrolein and silyl enol ether are utilized to perform Mukaiyama aldol reaction, sodium borohydride is used for reducing ketone into alcohol, and then pyridinium p-toluenesulfonate refluxes in a methylbenzene solutionto obtain compound shown in a formula 5; after cinnamyl aldehyde and an evans chiral aid are used for performing evans aldol reaction, diisobutyl aluminum hydride is used for reducing the cinnamyl aldehyde and the evans chiral aid at first, and then addition with metal indium activated 3-propylene bromine is performed to obtain compound shown in a formula 9; the compound shown in the formula 9 isresolved and purified for many times by kinetic resolution; the compound shown in the formula 9 and 2,2-diemthoxy propane can obtain fragment type 10 compound under the pyridinium p-toluenesulfonatecondition, the fragment type 10 compound and fragment type 5 compound can generate olefin metathesis reaction through a Grubbs secondary catalyst, and protecting groups of the fragment type 10 compound are removed under the hydrochloric acid condition to obtain Cryptofolione.