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 4-Bromo-1-indanone
15115-60-3

4-Bromo-1-indanone synthesis

12synthesis methods
3-(2-Bromophenyl)propionic acid

15115-58-9

4-Bromo-1-indanone

15115-60-3

General procedure for the synthesis of 4-bromoinden-1-one from 3-(2-bromophenyl)propionic acid: trifluoromethanesulfonic acid (3 equiv.) was slowly added dropwise at 0 °C to an anhydrous dichloromethane (1.0 mL) solution of 3-(2-bromophenyl)propionic acid (0.5 mmol) which was placed in a 12 mL Q-tube?pressure tube (provided by QLabtech). Subsequently, the reaction mixture was warmed to room temperature. A PTFE septum was placed on top of the reaction tube and sealed using the appropriate cap and pressure adapter. The sealed reaction tube was heated in an oil bath at 80°C. The progress of the reaction was monitored by thin layer chromatography (TLC) and gas chromatography-mass spectrometry (GC/MS) until the reactants completely disappeared. After completion of the reaction, the mixture was poured into ice water and extracted three times with dichloromethane. The organic phases were combined, dried with anhydrous sodium sulfate, filtered and concentrated under reduced pressure. Finally, the target compound 4-bromoinden-1-one was isolated and purified from the crude product by fast column chromatography.

-

Yield:15115-60-3 435 g

Reaction Conditions:

with aluminum (III) chloride in dichloromethane at 23 - 27; for 3 h;

Steps:

4-Bromo-2,3-dihydro-1H-inden-1-one

3-(2-Bromophenyl)propanoic acid (1) (550 g, 2.4 mol, 1 equiv) was dissolved in 1,2-dichloroethane (5.5 L). Thionyl chloride (437.8 mL, 6 mol, 2.5 equiv) was added to the solution and the mixture was refluxed for 24 hours. The reaction was cooled to room temperature and concentrated under reduced pressure. The residue was dissolved in methylene chloride (1 L) and added dropwise to a mechanically stirred suspension of anhydrous aluminum chloride (526.9 g, 3.96 mol, 1.65 equiv) in dichloromethane (1 L) while keeping the reaction temperature below 27° C. The reaction was stirred at room temperature for three hours before being quenched into a five gallon bucket which was half-full of ice. The resulting mixture was extracted with dichloromethane (3×3 L). The combined organic layers were washed sequentially with saturated brine (2 L) and saturated sodium bicarbonate (2 L). The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The resulting solid was dried overnight in a vacuum oven at 30° C. to give compound 2 (435 g, 86% yield) as an off-white solid.

References:

US9249239,2016,B2 Location in patent:Page/Page column 51

4-Bromo-1-indanone Related Search:

当涂县| 灵璧县| 德清县| 九龙坡区| 河间市| 丹寨县| 临高县| 普陀区| 饶平县| 富裕县| 红原县| 张家口市| 宜黄县| 牙克石市| 富宁县| 句容市| 云浮市| 石河子市| 松潘县| 紫金县| 乳源| 三河市| 新巴尔虎左旗| 黄陵县| 闽侯县| 体育| 视频| 布尔津县| 扎赉特旗| 肃宁县| 乌恰县| 曲松县| 洞口县| 叙永县| 高要市| 尤溪县| 平利县| 凤阳县| 嵩明县| 敦化市| 二连浩特市|