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 PHOSPHINE OXIDE, [2-[3,5-BIS [[(1,1-DIMETHYLETHYL) DIMETHYLSILY]OXY]-2-METHYLENECYCLOHEXYLIDENE]ETHYL]DIPHENYL-,[3S-(1Z,3A,5B0)]
81522-68-1

PHOSPHINE OXIDE, [2-[3,5-BIS [[(1,1-DIMETHYLETHYL) DIMETHYLSILY]OXY]-2-METHYLENECYCLOHEXYLIDENE]ETHYL]DIPHENYL-,[3S-(1Z,3A,5B0)] synthesis

14synthesis methods
-

Yield:81522-68-1 50%

Reaction Conditions:

Stage #1: Diphenylphosphine oxidewith potassium hydroxide;tetrabutylammomium bromide in tert-butyl methyl ether;water at 20; for 0.25 h;
Stage #2: <3S-(1Z,3α,5β)>-2-<3,5-bis<<(1,1-dimethylethyl)dimethylsilyl>oxy>-2-methylenecyclohexylidene>-1-chloroethane in tert-butyl methyl ether;water at 20; for 2.08333 - 2.16667 h;

Steps:

1 Preparation of 3S-(3α,5β,Z)-2-2-2-methylene-bis(1,1-dimethylethyl)dimethyl-silyl-oxy-cyclohexylidene-ethyl-diphenyl phosphine oxide

Example 1 Preparation of 3S-(3α,5β,Z)-2-2-2-methylene-bis(1,1-dimethylethyl)dimethyl-silyl-oxy-cyclohexylidene-ethyl-diphenyl phosphine oxide Potassium hydroxide (1.0 g, 17.97 mmole) was dissolved in water (0.5 mL) and was then added to a mixture of tetra-n-butylammonium bromide (TBAB) (1.16 g, 3.59 mmole) as phase transfer catalyst and diphenyl phosphine oxide (2.9 g, 14.37 mmole, prepared from chloro-diphenyl phosphine) in methyl t-butyl ether (MTBE) (40 mL) at room temperature. After stirring for 15 minutes, a solution of the chloro-compound (Z)-(1 S,5R)-1,5-bis-(tert-butyl-dimethyl-silanyloxy)-3-(2-chloro-ethylidene)-2-methylene-cyclohexane (5.0 g, 11.98 mmole) in MTBE (15 mL) was added drop-wise (during 5-10 min.). The reaction mixture was then stirred for 2 hours at room temperature. Thin Layer Chromatography (TLC) showed only a small amount of starting material (5-10%). The reaction product was diluted with MTBE (50 mL) and water (25 mL). The layers were separated and the organic layer was washed with water (25 mL) and brine (25 mL), dried with anhydrous Na2SO4, filtered, and concentrated under vacuum. The crude (6.0 g) was purified by column chromatography (EA: Hexane) to give 2.5g (~50%) of the desired phosphine oxide (94% desired by HPLC purity). This material was re-purified by column chromatography (EA: Hexane) to afford 1.7 g of pure material (1.7g, HPLC=96.04%). Identification and purity were verified by 1H NMR and HPLC. The remaining fractions were collected and added into the next batch.

References:

US2008/300427,2008,A1 Location in patent:Page/Page column 4

PHOSPHINE OXIDE, [2-[3,5-BIS [[(1,1-DIMETHYLETHYL) DIMETHYLSILY]OXY]-2-METHYLENECYCLOHEXYLIDENE]ETHYL]DIPHENYL-,[3S-(1Z,3A,5B0)] Related Search:

惠安县| 乌兰察布市| 揭阳市| 信丰县| 海南省| 简阳市| 启东市| 乌鲁木齐县| 慈溪市| 商河县| 南郑县| 宽甸| 柳林县| 黄平县| 南皮县| 宿州市| 监利县| 合川市| 霍山县| 工布江达县| 宝山区| 平潭县| 吐鲁番市| 无极县| 怀集县| 石泉县| 武冈市| 敖汉旗| 抚宁县| 双桥区| 高清| 大同县| 安丘市| 城固县| 黔西| 东乡县| 凤山市| 清河县| 寿阳县| 安庆市| 玛多县|