45results about How to "Moderate yield" patented technology

The invention relates to a synthesis method of tert-butyl-1, 7-diazaspiro [3.5] nonane-1-formate, and mainly solves the technical problem that no suitable industrial synthesis method exists at present. The method comprises the following seven steps: 1, reacting a compound 1 with ethyl malonate added into a solvent ethanol to obtain a compound 2; 2, reacting the compound 2 with lithium borohydridein tetrahydrofuran to obtain a compound 3; 3, reacting the compound 3 with p-toluenesulfonyl chloride in dichloromethane to obtain a compound 4; 4, adding cesium carbonate into the compound 4 in acetonitrile serving as a solvent for cyclization to obtain a compound 5; 5, adding magnesium chips into the compound 5 in methanol serving as a solvent for reduction to obtain a compound 6, 6, reacting the compound 6 with Boc anhydride in dichloromethane to obtain a compound 7, and 7, reacting the compound 7 with palladium on carbon in methanol to obtain a final compound 8.

The invention discloses a preparation method of palbociclib for treating breast cancer. The method comprises the following steps: 1) enabling N-cyclopentyl-2-methoxyl-3-cyan-4-methyl-5-acetyl-6-oxopiperidine-2-alkene and N-[5-(1-piperazinyl)-2-pyridyl] guanidine in the presence of N, N-Mes imidazolium salt to carry out a contact reaction to obtain 6-acetyl-8-cyclopentyl5-methyl-2-[[5-(1-piperazinyl)-2-pyridyl]amino]-5,6-dihydropyridino-[2,3-d]pyrimidine-7(8H)-ketone, wherein the temperature of the contact reaction is 85-100 DEG C; and (2) enabling 6-acetyl-8-cyclopentyl5-methyl-2-[[5-(1-piperazinyl)-2-pyridyl]amino]-5,6-dihydropyridino-[2,3-d]pyrimidine-7(8H)-ketone obtained in step 1) to carry out a dehydrogenation reaction in the presence of a dehydrogenation accelerant to generate palbociclib. The method is simple, is mild in condition and is capable of improving the yield and shortening the reaction time.

Novel processes for preparing arylsulfur pentafluorides are disclosed. Processes include reacting at least one aryl sulfur compound with a halogen and a fluoro salt to form an arylsulfur halotetrafluoride. The arylsulfur halotetrafluoride is reacted with a fluoride source to form a target arylsulfur pentafluoride.

The invention relates to 1,1-diacetate synthesis catalyzed by sulfonated cage-type mesoporous carbon. The method is characterized in that aldehyde and acetic anhydride are placed in a reactor according to a molar ratio of 1:1-3; a sulfonated cage-type mesoporous carbon catalyst is added, wherein 5-20mg of the sulfonated cage-type mesoporous carbon catalyst is added to each mole of aldehyde; the materials are stirred under room temperature until a reaction is sufficiently carried out; ethyl acetate with a volume 20-30 times that of the reaction liquid is added; the catalyst is removed by filtering; a filtrate is washed three times by using a saturated NaHCO3 water solution, and once by using water; an organic phase is dried by using anhydrous Na2SO4; the solvent is removed by reduced-pressure distillation under a pressure of 0.09MPa, such that a crude product is obtained; and re-crystallization or column chromatographic separation is carried out, such that 1,1-diacetate is obtained. Compared with existing 1,1-diacetate synthesizing method, the method provided by the invention has the advantages of short reaction time, high yield, mild reaction condition, recyclable catalyst, and the like. The method can be used for synthesizing 1,1-diacetate.

The invention relates to a brewing process of sweet sparkling apple wine. The process comprises the following steps: (1) soft-pressing juice taking by an extrusion method; (2) juice clarification; (3)low-temperature concentration and separation; (4) temperature-controlled fermentation; (5) pressure-maintaining low-temperature fermentation; (6) sugar-maintaining termination fermentation; and (7) clarification filtering treatment. The physicochemical indexes are as follows: the alcoholic strength is 11.5-12.0 (v/v)%, the reducing sugar content is greater than or equal to 95.0 g/L, the total acidity is 8.0-9.0 g/L, the free SO2 content is less than or equal to 50mg/L, the total SO2 content is less than or equal to 150mg/L, the volatile acid content is less than or equal to 0.8 g/L, and the pressure is 0.25-0.35 MPa. The process has the advantages that the juice is extracted through soft pressing, so that the influence of bitter substances on the aroma, taste and quality of the juice is reduced; the aroma and sugar of the fruit juice are concentrated through a low-temperature concentration technology; and through low-temperature pressure-maintaining fermentation and sugar-maintainingtermination fermentation, the finished wine is beautiful and light golden yellow. The finished wine is clear and transparent, bubbles are lasting and fine, and the finished wine has typical apple aroma and nectar aroma, strong fruity aroma, elegant and pure wine aroma, mellow and mellow taste, fullness, coordination, complexity, balance, and fragrant, fresh and lasting aftertaste.

The invention relates to a brewing process of mixed fragrance type sparkling sweet apple wine. The brewing process comprises the following steps: step 1, carrying out soft-pressing to take juice; steptwo, adjusting the acidity of lemon juice; step three, carrying out clarification of fruit juice; step four, carrying out concentration and separation at a low temperature; step five, carrying out temperature-controlled fermentation; step six, carrying out clarification and filtering; step seven, carrying out pressure-maintaining secondary fermentation; step eight, carrying out incomplete fermentation termination; step nine, carrying out low-temperature ageing; and step ten, carrying out clarification and filtration treatment under the conditions of setting physical and chemical indexes as follows: 11.5 to 12.0 (v/v) percent of the alcoholic strength, reducing sugar being greater than or equal to 95.0 g/L, total acidity of 8.0 to 9.0 g/L, free SO2 being less than or equal to 50mg/L, totalSO2 being less than or equal to 150mg/L, volatile acid being less than or equal to 0.8g/L, and the pressure of0.25 to 0.35 MPa. The brewing process has the following advantages: after the process operation, the influence of easy oxidation and browning of the apples after juicing on the aroma, taste and quality of the juice is reduced; the acidity of the apple juice is adjusted by lemon juice, sothat the complexity of the fragrance and the taste of the apple juice are increased; the oxidation resistance of the apple juice is improved; with the low-temperature concentration technology, the pressure-maintaining secondary fermentation technology, the incomplete fermentation termination technology and the low-temperature ageing technology with yeast paste, the yeast fragrance is enhanced while the wine fragrance contains the fine apple fragrance and elegant lemon fragrance, so that the aroma richness is improved, the taste is more mellow and complex, and the sweetness is pure and clean without sweet greasy feeling.

The invention relates to novel cell-penetrating fluorescent dyes with secondary alcohol functionalities having one of the following general formulae I-III and 4: The invention also relates to the use of these compounds for optical microscopy and imaging techniques.

The invention relates to camptothecin, in particular relates to homocamptothecin compounds and a synthesis method thereof, and mainly solves the technical problems of poor solubility and bioavailability of homocamptothecin in the prior art. Structural formulas of the homocamptothecin compounds are as shown in I and II, and the homocamptothecin compounds comprise racemic compounds and (S)-and (R)-stereisomers corresponding to the racemic compounds. The invention specifically relates to derivation of 10-hydroxyl homocamptothecin compound, the 10-hydroxyl homocamptothecin is used as a mother nucleus for synthesis of a series of homocamptothecin ester and amide compounds. The invention provides a new synthetic route, and according to the path, a full synthesis ring enlargement method is not needed, and protection and deprotection are not needed.

The invention discloses an improved method for preparing penfuridol, comprising the following steps: using 4, 4-bis (4-fluorophenyl) butyric acid as a starting material, carrying out reduction synthesis to synthesize an intermediate I [4, 4-bis (4-fluorophenyl)-1-butanol]; carrying out esterification with a sulfonyl chloride compound to synthesize an intermediate II [4, 4-bis (4-fluorophenyl)-1 (4-methyl-phenyl)-butyl sulfonate] or [4, 4-bis (4-fluorophenyl)-1-methyl-butyl sulfonate]; and condensing with pipradrol to obtain penfuridol. According to the preparation method, 4, 4-bis (4-fluorophenyl) butyric acid is used as a raw material, penfuridol is obtained through a reduction reaction, an esterification reaction and a condensation reaction, the total yield is 81.3%, the whole process isconvenient to operate and mild in reaction, the obtained product is high in yield and purity, and the preparation method is more economical and more suitable for industrial application. The technicalproblems that an existing method is low in yield and poor in purity are solved. The reaction general formula is as shown in the specification.

The invention discloses a synthesis method of 1H-pyrrolo[2,3-b]pyridine-2-boronic acid pinacol ester, and belongs to the field of medicinal chemistry. The synthesis method comprises the following steps: reacting 7-azaindole serving as a raw material with di-tert-butyl dicarbonate to synthesize 1H-pyrrolo[2,3b]pyridine-1-carboxylic acid tert-butyl ester, reacting the 1H-pyrrolo[2,3b]pyridine-1-carboxylic acid tert-butyl ester with n-butyl lithium and 1,2-dibromotetrafluoroethane at low temperature to synthesize 2-bromo-1H-pyrrolo[2,3-b]pyridine, synthesizing 2-bromo-1H-pyrrolo[2,3-b]pyridine-1-carboxylic acid tert-butyl ester, removing the protective group to obtain 2-bromo-1H-pyrrolo[2,3-b]pyridine, and reacting 2-bromo-1H-pyrrolo[2,3-b]pyridine with bi-pinacol borate under the catalytic action of transition metals to obtain the target product. The raw materials and reagents are cheap and easy to obtain, reaction conditions are mild, the safety is high, the cost is low, and the preparation method is easily applied to industrial batch production.