69 results about "P-nitrobenzoyl chloride" patented technology

The invention relates to a preparation method of folic acid. The process steps are as follows: firstly, the intermediate product N-p-aminobenzoyl glutamic acid is prepared by using p-nitrobenzoyl chloride and sodium glutamate; Guanidine and sodium methoxide were used to prepare the intermediate product 6-hydroxy-2,4,5-triaminopyrimidine sulfate; finally, the above two intermediate products were used to prepare crude folic acid, which was purified to obtain pure folic acid. The beneficial effects of the invention are that the production cost is greatly reduced, the product efficiency is improved, and the pollution to the environment is reduced.

The present invention relates to fluorine-containing asymmetric aromatic diamine, a preparation method and an application thereof in the synthesis of polyimide. The compound has a constitutional formula as shown in the right. The preparation method comprises the following steps: (1) 2, 6-dimethyl phenol, paranitrobensoyl chloride and alchlor have catalytic reaction in an organic solvent to prepare (4'-hydroxy-3', 5'-dimethyl benzene)-(4-nitrophenyl) ketone; (2) the (4'-hydroxy-3', 5'-dimethyl benzene)-(4-nitrophenyl) ketone reacts with 2-chlorine-5-nitro trifluorotoluene with alkaline, to prepare (3', 5'-dimethyl-4'-(4''-nitro-2''-trifluoromethyl phenoxy) benzene)-(4-nitrophenyl) ketone; (3) the prepared product in the second step is reduced by reducing agent with organic solvents and catalysts; thus the fluorine-containing asymmetric aromatic diamine can be prepared. The fluorine-containing asymmetric aromatic diamine can be used for preparing fluorine-containing polyimide. The fluorine-containing asymmetric aromatic diamine prepared in the method has high purity and can keep stable at the room temperature; the polyimide made of the fluorine-containing asymmetric aromatic diamine has excellent solubility, film forming capability, optical transparency, mechanical properties and heat resistance.

The invention provides 2-amino-fluorene containing an ester group and a preparation method thereof. The preparation method includes reacting 2-hydroxy-fluorene with p-nitrobenzoyl chloride at a room temperature for 1-5 hours, wherein the mass ratio of the 2-hydroxy-fluorene and the p-nitrobenzoyl chloride is 1:(2-2.2), subjecting the mixture to a reaction under a reflux condition for 10-24 hours to obtain 2-nitrofluorene containing the easter group; and subjecting the 2-nitrofluorene containing the easter group to reduction through hydrazine hydrate to obtain the white 2-amino-fluorene containing the ester group in the presence of a catalyst for 24-60 hours of reflux reaction, wherein the mass ratio of the 2-nitrofluorene containing the easter group and the hydrazine hydrate is 1:(3.2-4.8). According to the 2-amino-fluorene containing the ester group, flexibility of molecules is improved while thermal performance cannot be reduced greatly due to the induction of the ester group; and the 2-amino-fluorene containing the ester group can serve as a raw material for a curing agent for epoxy resin, polyimide and benzoxazine.

The invention provides a method for synthesizing p-aminobenzamide, comprising the steps of: 1) taking a container, adding p-nitrobenzoic acid, triphosgene and a solvent, after the reaction is completed, collecting the solvent to obtain p-nitrobenzoyl chloride; ) take another reaction vessel, add ammonia and phase transfer catalyst, drop p-nitrobenzoyl chloride toluene solution to obtain p-nitrobenzamide; 3) take the reaction kettle, add p-nitrobenzamide, and add water, Catalyst, obtains described p-aminobenzamide. In the method, the amount of raw materials used is small and the reaction speed is fast. After the hydrogen chloride gas produced by the reaction is absorbed into hydrochloric acid by water, it can be used for other purposes, which effectively reduces the production cost. In the reduction reaction, the iron powder method is replaced by the hydrogenation method, so that the production The cost is reduced, no solid waste is generated, the labor load is greatly reduced, the process is environmentally friendly, and the economic benefit is good.

The present invention relates to a preparation method of folic acid, the technical steps of which are as follows: firstly, p-nitrobenzoyl chloride and sodium glutamate are used to prepare for a mediumproduct N-p-amino-benzoyl glutamic acid; then, methyl cyanoacetate, guanidine nitrate and sodium methoxide are used to prepare for the medium product 6-hydroxyl-2, 4, 5-triamino pyrimidine sulfate; finally, the two kinds of medium products are used to prepare for a crude product of the folic acid which is refined to obtain the pure product of the folic acid. The present invention has the beneficial effects of reducing the production cost greatly, improving the product efficiency and reducing the pollution to the environment.

The invention provides a refining process of a paranitrobenzoyl chloride intermediate. The refining process comprises the following steps that a xylene solution is added to a reaction kettle, then paranitrotoluene is added to the xylene solution, air is fed into the reaction kettle, and sodium dichromate is added to the reaction kettle; concentrated sulfuric acid is drop added to the reaction kettle; stirring of the reaction kettle is stopped, an NaOH solution is added to the reaction kettle until the PH of the reaction kettle is 7; the solution is transferred to a rectifying kettle, the heated solution is heated, nitrogen is fed for exhausting, then the solution after exhausting is cooled, and crystallization is performed, so that the paranitrobenzoyl chloride intermediate is obtained. With the adoption of the production process, the process is simpler, control is easy, the production amount of impurities is reduced in the production process, the reaction time is saved, and accordingly, the production efficiency is improved.

The invention discloses a preparation method of p-amino benzamide glutamic acid. The preparation method comprises the following steps of (1) adding 180g / ml glutamic acid and a paranitrobenzoyl chloride condensate into a water solution, and stirring until the 180g / ml glutamic acid and the paranitrobenzoyl chloride condensate are sufficiently dissolved to prepare a p-amino benzamide glutamic acid water solution with the weight ratio of 35%; (2) regulating the pH value to 7.3, adding 52g / ml ammonium chloride, heating to 55 DEG C, adding 63g / ml gray cast iron powder, heating to 75 DEG C, pre-corroding for 2.5 hours, heating to 85 DEG C, and preserving the heat for 3.5 hours; and (3) filtering to remove iron mud, washing with distilled water, adding carbon for discoloring, crystallizing, carrying out suction filtration, washing, and drying to obtain a finished product of p-amino benzamide glutamic acid. By using the preparation method of p-amino benzamide glutamic acid, disclosed by the invention, the reaction conversion rate is increased, and the environment pollution is reduced.

The invention relates to the technical field of preparation method of tetracaine hydrochloride. The preparation method comprises the preparation steps: carrying out a reaction of p-nitrobenzoyl chloride (2) and 2-dimethylamino-1-ethanol (3) to generate p-nitrobenzoic acid-2-dimethylamino ethyl (4), reducing the compound (3) to obtain p-aminobenzoic acid-2-dimethylamino ethyl (4), generating pontocaine (7) from a compound (5) and 1-bromobutane (6) under alkaline conditions, and finally carrying out a reaction of the pontocaine (7) with HCl to generate tetracaine hydrochloride (1).

The present invention discloses a low-oxygen-responsive polyamino acid-PEG stereo drug-loaded micelle and a preparation method thereof. The preparation method comprises the following steps: firstly selecting 2-nitroimidazole and dibromo neopentyl glycol to conduct reaction under catalysis of cesium carbonate to obtain 2,2-bis[(2-nitro-1H-imidazole-1-yl)methyl]-1,3-propylene glycol, then conductingacyl halide with p-nitrobenzoyl chloride in presence of triethylamine to obtain 2,2-bis[(2-nitro-1H-imidazole-1-yl)methyl]propane-1,3-diylbis(4-nitrophenyl)carbonate, then conducting reaction with paclitaxel under catalysis of N,N-diisopropylethylamine, then adding poly L-amino acid-PEG or poly D-amino acid-PEG to respectively obtain bis 2-nitroimidazole-paclitaxel-poly L amino acid-PEG and bis 2-nitroimidazole-paclitaxel-poly D amino acid-PEG, respectively, finally mixing the two materials at equal amount in a PBS buffer, conducting homogenization at high speed, and conducting extruding witha filter membrane with a pore size of 100 nm to obtain a finished product. The prepared drug-loaded micelle has high encapsulation efficiency and also low-oxygen-responsive characteristics, can be effectively accumulated in tumor tissues to achieve a very good antitumor effect, and reduces distribution of drugs in other normal tissues to reduce toxic and side effects.

The invention discloses a preparation method of N-tert-butyl-4-aminobenzamide. The preparation method of the N-tert-butyl-4-aminobenzamide comprises the steps that a condensation reaction is carried out on p-nitrobenzoyl chloride and tert-butylamine to obtain N-tert-butyl-4-nitrobenzamide, and further, the N-tert-butyl-4-aminobenzamide is obtained by catalytic hydrogenation, wherein the condensation reaction is carried out in the presence of a mixed solvent, the mixed solvent is toluene-water, and the condensation reaction comprises the steps that reaction is carried out at 5-10 DEG C for 0.5-2 h, and then reaction is carried out at room temperature for 0.5-2 h, and finally heating is carried out to reflux for reaction for 1-4 h. According to the condensation reaction of the preparation method of the N-tert-butyl-4-aminobenzamide, toluene and water are used as the mixed solvent, then reaction is carried out at room temperature for a certain period of time, and then heating is carried out to reflux to continue the reaction for a certain period of time, so that the yield of the condensation reaction can be significantly increased; and the reduction reaction avoids the use of hydrazine hydrate, and environmental-protection is achieved.

The invention belongs to the field of chemical synthesis and relates to a preparation technology of a PET (Polyester Terephthalate) imaging agent, in particular to a synthesis method for a diphenyl-substituted oxadiazole derivative of a labeled precursor of a positron medicament Abeta plaque agent, i.e. 4-(3-(4-hydroxyphenyl)-1,2,4-oxadiazole-5-yl)-aniline and a reference substance of 4-(3-(4-hydroxyphenyl)-1,2,4-oxadiazole-5-yl)-N-methylaniline thereof. In the invention, the method comprises the following steps of: condensing cyanobenzene and hydroxylamine hydrochloride as raw materials to obtain p-methoxybenzamidoxime; cyclizing the p-methoxybenzamidoxime and paranitrobenzoyl chloride to obtain 3-(4-methoxyphenyl)-5-(4-nitrophenyl)-1,2,4-oxadiazole; reducing the 3-(4-methoxyphenyl)-5-(4-nitrophenyl)-1,2,4-oxadiazole and removing hydroxymethoxyl to obtain the labeled precursor; and methylating a reduzate of amine and then removing hydroxymethoxyl to obtain the reference substance. By adopting the method, the yield of obtaining the labeled precursor of a target product reaches 20%, and the whole reaction process has mild condition and is easy to operate.