Identification Study on Cryptotympana pustulata Ecdysis Based on 3D Depth of Field Synthesis Technology / 中国药房

OBJECTIVE：To establish the rapid field identification method of Cryptotympana pustulata ecdysis. METHODS ： 3D depth of field synthesis technology was used to identify 50 batches of C. pustulata ecdysis and its adulterants from the length of beak ，size and protrusion degree of upper labial base ，the protrusion degree of the lower labial base ecdysis and the color of its upper transverse groove ，the number and shape of main and lateral spines on the foot ，significance of abdominal valves ，the number of webs ，the number and shape of side plates ，the number of tergum rings ，terminaliae，etc. RESULTS ：Among 50 batches of samples ，S1-S5，S26-S30，S36-S50 were C. pustulata ecdysis；S21-S25 was adulterants of C. pustulata ecdysis after weight gain ；S31-S35 was adulterants of C. pustulata ecdysis after extraction ；S6-S20 were ecdysis from Tibicen flammatus ，C. flammatta，Lyristes pekinensis ，all of which were adulterants. The main distinguishing feature of C. pustulata ecdysis and its adulterants was that abdomen and ventral surface of C. pustulata ecdysis were triangular ，and the abdomen and ventral surface of other species was nearly parallel ；the valve of C. flammatta ecdysis was obvious ，but those of other varieties were not obvious ；the lateral appearance of terminaliae of C. flammatta ecdysis was sharper than those of other species ；there was an acute angle between the front foot accessory thorns and the end thorns of the T. flammatus ecdysis，and an obtuse angle between the front foot accessory thorns and the end thorns of the L. pekinensis ecdysis. CONCLUSIONS ：The method is simple ，reliable and suitable for rapid field identification of C. pustulata ecdysis and its adulterants.

Study on the Optimization of Synthesis Technology of 4-biphenylacetic Acid / 中国药房

OBJECTIVE:To optimize the synthesis technology of 4-biphenylacetic acid,and to provide technology support to meet the market demand of 4-biphenylacetic acid raw material. METHODS:The synthesis route of 4-biphenylacetic acid from biphenyl by Friedel-Crafts reaction,ketal reaction,rearrangement reaction and hydrolysis was optimized and improved. The effects of different Friedel-Crafts reaction solvents (petroleum ether,dichloromethane,1,2-dichloroethane),ketal reaction ethanol (ethanediol, 1,3-propanediol, dimethyltrimethylene glycol, pentaerythritol), rearrangement reaction catalyzer (zinc biphenyl acetate,zinc oxide,zinc caprylate,zinc acetate) and refined solvent (isopropanol,95% isopropanol,ethanol,acetone,ethyl acetate) on synthesis technology were investigated. The optimal synthesis technology was screened with the purity and yield of intermediate or 4-biphenylacetic acid. RESULTS:The petroleum ether as Friedel-Crafts reaction solvent,ethylene glycol as ketal reaction ethanol,zinc diphenylacetate as rearrangement catalyst and 95% isopropanol as refining solvent were used for the preparation to obtain better effects. The yield of key intermediate 2′-chloroacetophenone reached above 95%. The purity of refined 4-biphenylacetic acid reached 99.9%;the content of single impurity was less than 0.1%;the total yield reached over 70%. CONCLUSIONS:The optimal synthesis technology of 4-biphenylacetic acid has the advantages of simple operation,mild and controllable reaction conditions,low cost,greener reagents and higher safety,and is suitable for industrial production. The purity and yield of the products are in high level and in line with the standards of European Pharmacopoeia and the Japanese Pharmacopoeia.

Improvement of the Synthesis Technology of 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2 (1H)-ketone / 中国药房

OBJECTIVE:To improve the synthesis technology of 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2 (1H)-ketone. METHODS:Using 2-methyl-4(3H)-quinazolone as starting material,the synthesis technology of 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2(1H)-ketone was improved by clorination, nucleophilic substitution, diarylamine alkylation and nitro reductive cyclization. The yield of it was investigated. RESULTS:The structure of 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2(1H)-ketone had been verified by 1H-NMR and ESI-MS. The yield was 43.5%and improved by 23.3% compared to 20.2% before improvement. CONCLUSIONS:Improved technology is simpler and milder, which is suitable for the batch preparation of laboratory study.

Improvement of Synthesis Technology for Sodium Picosulfate / 中国药房

OBJECTIVE:To improve the synthesis technology of sodium picosulfate. METHODS:The synthesis technology of sodium picosulfate was improved by changing reaction solvent,charging sequence,refined method and formation of crystal water. Using phenol as raw material,it was condensed with 2-pyridinecarboxaldehyde to achieve 4,4′-(pyridin-2-ylmethylene)diphenol, and its yield rate was investigated. Sodium picosulfate was obtained after esterification,salification,formation of crystal water, and then its purity was determined. RESULTS:The yield rate of key intermediate 4,4′-(pyridin-2-ylmethylene) diphenol reached above 88%,and the purity of refined products reached over 99.5%. Sodium picosulfate monohydrate was stable,and the content of single impurity was less than 0.1%. CONCLUSIONS:The improved technology is simple with mild conditions,and suitable for large-scale production.