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 1,1'-Sulfonylbis[4-(prop-2-en-1-yloxy)benzene
41481-63-4

1,1'-Sulfonylbis[4-(prop-2-en-1-yloxy)benzene synthesis

3synthesis methods
The preparation of 1,1'-Sulfonylbis[4-(prop-2-en-1-yloxy)benzene is as follows:2400g water, 216g caustic soda lye of 48% strength, 600g 4,4'-dihydroxydiphenyl sulfone and 204g Allyl chloride were mixed and the reaction was carried out at 55-60°C and autogenously generated pressure of 0.8-1. Okg/cm2 for 8 hours. 204g caustic soda lye of 48% strength was added in the reaction mixture, and maintained for 1 hour at 80°C thereafter filtered at 80°C to remove 4,4'-diallyloxydiphenyl sulfone. Further, the filtrate solution was treated with 5g activated carbon and 5g sequestering agent at 85- 90°C. The pH of filtrated solution was adjusted to 8.9 with 20% sulfuric acid and cooled to 35°C. The precipitate was separated by filtration and slurred in water. The pH was adjusted to 4.94 with 20% sulfuric acid and the precipitate was separated by filtration, and washed with water and dried to obtain 615g the product 4-allyloxy 4'-hydroxydiphenyl sulfone of 96% purity. The yield was 93.5% with respect to 4,4'-dihydroxydiphenyl sulfone. The wet cake of 4,4'-diallyloxydiphenyl sulfone was slurred in 100g of 5%w/v aqueous solution of sodium hydroxide and refluxed for 1 hour, then cooled to 80°C. The precipitate was filtered, washed with water and dried to obtain 45g of 4,4'-diallyloxy diphenyl sulfone of 91.9% purity. The yield was 6% with respect to 4,4'-dihydroxydiphenyl sulfone. pH of the mother liquor obtained after separation of 4-allyloxy 4'-hydroxydiphenyl sulfone, was adjusted to 4.5 with 20% sulfuric acid. The precipitate was separated by filtration, washed with water and dried to obtain 33g of 4,4'-dihydroxydiphenyl sulfone of 87.9% purity. The conversion of 4,4'-dihydroxydiphenyl sulfone was 94.50%.; 595g of 4-allyloxy 4'-hydroxydiphenyl sulfone of 96% purity was dissolved in 230g of 48% strength caustic soda lye and 1000g water, treated with 5g activated carbon and 5g sequestering agent at 85-90°C. The slurry was filtered and pH of the filtrate was adjusted to 8.95 with 20% sulfuric acid and then cooled to 35°C. The precipitate was separated by filtration, slurried in water and the pH was adjusted to 5.0 with 20% sulfuric acid. The slurry was filtrated and the precipitate was washed with water and dried to obtain 563g of 4- allyloxy 4'-hydroxydiphenyl sulfone of 99.273% purity.

QQ截圖20221115115918.png

-

Yield: 94%

Reaction Conditions:

Stage #1:4,4'-sulfonediphenol with potassium carbonate in acetone for 1 h;Inert atmosphere;Reflux;
Stage #2:allyl bromide in acetoneReflux;Inert atmosphere;

Steps:

D. General procedure for the allylation and Claisen rearrangement of bisphenol derivatives
General procedure: In a three-neck round-bottom flask the bisphenol derivative (1a-c) and potassium carbonate (0.9-1.5 equivalents per hydroxy group) were dissolved in acetone (approx. 10 wt% regarding the bisphenol component). After heating the white suspension to reflux for 60 minutes under a nitrogen atmosphere, allyl bromide 6 (1.3-1.5 equivalents per hydroxy group) was added through a dropping funnel. The mixture was refluxed until the reaction was completed (as monitored by TLC). Then deionized water was added and extracted three times with diethylether. The combined organic extracts were washed three times with 1N NaOH-solution and brine, dried over anhydrous MgSO4, filtered and concentrated under reduced pressure.

References:

Reinelt, Sebastian;Tabatabai, Monir;Fischer, Urs Karl;Moszner, Norbert;Utterodt, Andreas;Ritter, Helmut [Beilstein Journal of Organic Chemistry,2014,vol. 10,p. 1733 - 1740] Location in patent:supporting information

1,1'-Sulfonylbis[4-(prop-2-en-1-yloxy)benzene Related Search:

万州区| 灯塔市| 海晏县| 江源县| 台江县| 磐石市| 平阴县| 辽源市| 锡林郭勒盟| 长顺县| 虹口区| 柘城县| 营山县| 奉新县| 宜君县| 红桥区| 定日县| 东兰县| 庐江县| 江西省| 东乌| 霍城县| 马公市| 广汉市| 怀远县| 宁武县| 顺昌县| 民丰县| 鄂伦春自治旗| 罗山县| 林芝县| 马鞍山市| 吐鲁番市| 宁国市| 泰安市| 石柱| 周宁县| 武功县| 海晏县| 浑源县| 醴陵市|