一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 3,4,5,6-Tetrachloro-2-cyanobenzoic acid ammonium salt
34643-39-5

3,4,5,6-Tetrachloro-2-cyanobenzoic acid ammonium salt synthesis

1synthesis methods
-

Yield:-

Reaction Conditions:

with ammonia;water in xylene at -4 - 85; for 6 h;Product distribution / selectivity;

Steps:

1.b; 5; 6

352 gm of TCPC solution obtained in step 1 (a) in the form of organic (xylene) layer was added drop by drop in a three necked round bottom flask containing 633 gm 25% liquor ammonia at molar ratio Jj9. Maintained at a temperature of 4.8°C. The flask was placed in an ice bath containing brine solution at temperature between -2°C to -4°C. The reaction mixture was allowed to stand for 60 minutes in the cold bath. The temperature was periodically checked to ensure that the temperature of the reaction mixture did not exceed 50C. Then the flask was removed from the bath and the temperature was slowly raised up to 500C in 1 hour time. The flask was further gradually heated to 85°C and stirred at this temperature for 4 hours. A hazy reaction mass was obtained. This mass was filtered in a Buchner funnel containing filter paper. Wet cake obtained was washed with 200 ml xylene. Xylene washed cake was dissolved in hot water at 800C to form a clear solution; to this solution, 100 ml of xylene was added. The reaction solution was stirred for 30 minutes at 800C and phase separation was seen in the flask in which the organic layer was at the top. Xylene layer was sent for recycling and the aqueous layer was transferred to an ice bath at 50C. Ammonium salt of TCCBA were precipitated as white shiny crystals. These crystals were separated by filtration. 286 gm of ammonium salt of TCCBA was obtained. This material was dried in tray dryer at 1000C for 8 hours.; Example 5; The process was carried out as per the Example 1 upto step (a). On step (b), 1 liter of ethyl alcohol was used as organic solvent instead of dimethyl formamide (DMF). The resultant white crystals of TCCMB was 205 gm having purity 95.0% having melting point of 84.5°C was obtained. The HCB content was measured on gas chromatogram and was found to be 7 ppm.; Example 6; The process was carried out as per the Example 1 upto step (a). On step (b), 1 liter of methyl alcohol was used as organic solvent instead of dimethyl formamide (DMF). The resultant white crystals of TCCMB was 204 gm having purity 96.0% having melting point of 84.6°C was obtained. The HCB content was measured on gas chromatogram and was found to be 6 ppm.

References:

WO2008/96371,2008,A1 Location in patent:Page/Page column 13-16

3,4,5,6-Tetrachloro-2-cyanobenzoic acid ammonium salt Related Search:

齐河县| 微博| 修文县| 莱阳市| 平阴县| 衡南县| 平邑县| 湖南省| 汤阴县| 寿阳县| 二连浩特市| 迁安市| 临邑县| 泗洪县| 牟定县| 绥滨县| 西藏| 莱芜市| 渭源县| 探索| 仙游县| 黄陵县| 太谷县| 岳阳市| 高阳县| 陵川县| 沂源县| 汉中市| 秦皇岛市| 巫溪县| 美姑县| 锡林浩特市| 克什克腾旗| 建水县| 喀什市| 库尔勒市| 永丰县| 肇东市| 兰西县| 鹤庆县| 庐江县|