- A+
AlCl3/CH3CN和AlBr3/CH3CN是【Bull. Chem. Soc. Jpn., 1995, 68, 2033】一类常用的去甲基化方法，其操作类似BBr3的使用，只是一般反应温度在0℃到室温。另外加入硫化物，由于硫的亲核性更强，可以增加反应活性。AlBr3/EtSH,AlCl3/EtSH, AlCl3/HSCH2CH2SH体系的活性很高，分子中酯、醛、酮、双键不稳定，但酯在AlCl3/EtSH/CH2Cl2体系相对稳定。
反应机理
加入硫代物
反应实例
Typical Procedure. To dichloromethane (1 mL) or CH3CN (1 mL) wasadded aluminum chloride (3.0 mmol) at 0 ℃. Theresulting solution was warmed to room temperature, and the ether (1.0 mmol) wasadded with stirring. After being stirred for 3-12 h, the reaction mixture was pouredinto water, acidified with dilute HC1, and extracted with dichloromethane. Theorganic layer was treated as usual to give a crude product. Chromatography over a silica gelcolumn gave the desired product.
【Y. Kawamura, H.Takatsuki, F. Torii, and T. Horie, Bull. Chem. Soc. Jpn., 1994,67, 511.】
General Procedure for Demethylation. To a stirredsolution of aluminum halide in ethanethiol cooled in an ice-water bath wasadded the substrate.The reaction was monitored by TLC (aluminum halide was quenched bymethanol in the capillary). The reaction mixture was poured into water,acidified with dilute HC1, and extracted with dichloromethane. The organiclayer was shaken with brine, dried (Na2SO4), filtered,and then evaporated to leave a crude material, which was purified bychromatography over a silica gel column.
AlCl3/EtSH/CH2Cl2体系：To a mixture of dry ethanethiol (1 mL) and dichloromethane (1 mL) was added aluminum chloride (0.40 g, 3.0 mmol) at 0 oC. The resulting solution was warmed to room temperature,and the ether (0.194 g,1.0 mmol) was added with stirring. After being stirred for 9.5 h, the reactionmixture was poured into water, acidified with dilute HCl, and extracted with dichloromethane.The organic layer was treated as usual to give a crude product.Chromatography over a silica gel column gave the desired product (0.157 g, 95.5%) identical with anauthentic sample.
AlCl3/EtSH 体系：To a solutionof aluminum chloride (47 mg, 0.35 mmol) in dry ethanethiol (1 mL) was added the ether (11 mg, 0.03mmol) at 0 oC. After being stirred for 2.5 h at 0 oC, the reactionmixture was poured into water and extracted with dichloromethane. The usual workup of theorganic layer gave the product: 7.5 mg (81.5%).
【 M. node, K.Nishide, K. Fuji and E. Fujita, J. Org. Chem. 1980, 45,4275. 】
В этом источнике вы обнаружите подробную информацию о программе лояльности: 1win партнерская программа.
У нас представлены все аспекты взаимодействия, правила присоединения и ожидаемые выплаты.
Каждая категория четко изложен, что помогает быстро понять в аспектах процесса.
Есть также вопросы и ответы и полезные советы для новых участников.
Контент дополняется, поэтому вы смело полагаться в актуальности предоставленных материалов.
Этот ресурс станет вашим надежным помощником в освоении партнёрской программы 1Win.
The site offers you the chance to find professionals for temporary high-risk jobs.
Visitors are able to securely arrange services for specific situations.
All workers are trained in handling critical tasks.
rent a hitman
The website offers discreet arrangements between requesters and contractors.
If you require urgent assistance, the site is the perfect place.
List your task and get matched with the right person now!
1xBet Promotional Code - Special Bonus maximum of $130
Enter the 1xBet bonus code: Code 1XBRO200 when registering on the app to access exclusive rewards provided by One X Bet for a welcome bonus as much as 100%, for sports betting along with a $1950 with 150 free spins. Launch the app then continue by completing the registration steps.
This 1xBet bonus code: 1XBRO200 gives a great sign-up bonus for first-time users — 100% as much as $130 during sign-up. Bonus codes serve as the key to obtaining extra benefits, also One X Bet's promotional codes aren’t different. By using such a code, bettors have the chance of various offers throughout their journey in their gaming adventure. Although you aren’t entitled for the initial offer, One X Bet India ensures its loyal users are rewarded through regular bonuses. Visit the Offers page on their website frequently to keep informed on the latest offers designed for existing players.
1xbet promo code for registration
Which 1XBet promotional code is presently available today?
The promo code relevant to 1xBet equals Code 1XBRO200, enabling novice players joining the bookmaker to access a bonus worth $130. To access unique offers pertaining to gaming and bet placement, kindly enter this special code concerning 1XBET during the sign-up process. In order to benefit of this offer, potential customers must input the promo code Code 1xbet at the time of registering step to receive a 100% bonus applied to the opening contribution.