- Green synthesis method for 1,2-bi(trialkyl siloxy) cyclohexene
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The invention relates to a green synthesis method for 1,2-bi(trialkyl siloxy) cyclohexene. The method comprises the step of causing 1,2-cyclohexanone, bi(trialkyl silicon) sulphate and reactive metalreact in an inert solvent, thereby acquiring 1,2-bi(trialkyl siloxy) cyclohexene. The bi(trialkyl silicon) sulphate is prepared according to the steps of preparing hexalkyl disiloxane by dehydrating by-product trialkyl silanol in consequent reaction and then continuing to react with concentrated sulfuric acid. The environmental issue of siloxane effluent is completely solved through the recyclingof silicon protecting group; the produced solid waste has a single component and can be prepared into byproduct for sale after simple treatment; the emission of three wastes is less; the technology isenvironment-friendly.
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Paragraph 0070; 0072-0077
(2018/12/14)
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- 1. 2 - double-trimethyl silicon oxygen radical link hexene and its preparation process
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The invention belongs to the field of chemical material production, and especially relates to 1,2-bis(trimethylsilyloxy)cyclohexene, and a preparation method thereof. Preparation chemical equation of 1,2-bis(trimethylsilyloxy)cyclohexene is represented by
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Paragraph 0018; 0023; 0025-0030; 0032-0044
(2017/10/07)
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- Chemoselective activation of trimethylsilyl enol ether functionalities in the presence of silyl-protected alcohols by trimethylsilyl-nonaflyl exchange
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Trimethylsilyl enol ethers bearing trialkylsilyl-protected hydroxy groups were converted into synthetically valuable bifunctional alkenyl nonaflates under the action of nonafluorobutane-1-sulfonyl fluoride combined with potassium fluoride in the presence
- Boltukhina, Ekaterina V.,Sheshenev, Andrey E.,Lyapkalo, Ilya M.
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experimental part
p. 3507 - 3515
(2011/12/04)
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- Cu(II)-catalyzed acylation by thiol esters under neutral conditions: Tandem acylation-wittig reaction leading to a one-pot synthesis of butenolides
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The first catalytic acylation of alcohols with a thiol ester present in Wittig reagents under neutral conditions catalyzed by the Cu(II) salt through a push-pull mechanism is reported. Furthermore, a new methodology for the one-pot lactonization of acyloins by a copper catalyst is developed. The synthetic utility of this method for the synthesis of natural products is shown.
- Matsuo, Kazumasa,Shindo, Mitsuru
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supporting information; experimental part
p. 5346 - 5349
(2011/01/05)
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- Fancy bioisosteres: Synthesis and dopaminergic properties of the endiyne FAUC 88 as a novel non-aromatic D3 agonist
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Enlargement of the π-electronic system of the non-aromatic D3 agonist FAUC 73 led to dopaminergic endiynes of type 1 being synthesized via the bromovinyl triflate 7a as a key intermediate when palladium catalyzed coupling reactions were exploited for the
- Lenz, Carola,Haubmann, Christian,Hübner, Harald,Boeckler, Frank,Gmeiner, Peter
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p. 185 - 191
(2007/10/03)
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- Hypervalent λ(n)-iodane-mediated fragmentation of tertiary cyclopropanol systems
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The oxidation of tertiary cyclopropyl silyl ethers with hypervalent λ(n)-iodanes caused fragmentation which produced alkenoic acids or esters.
- Kirihara, Masayuki,Yokoyama, Satoshi,Kakuda, Hiroko,Momose, Takefumi
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p. 13943 - 13954
(2007/10/03)
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- Convenient preparation of metals deposited on solid supports and their use in organic synthesis
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'High-surface alkali metals' can be conveniently prepared via deposition of corresponding metals on various supports such as sodium chloride, polyethylene, polypropylene and cross-linked polystyrene from their solutions in liquid ammonia. Alkali metals deposited on polymeric supports can be stored in form of stable suspensions in inert solvents and used for the acyloin and Dieckmann condensations and for preparation of organolithiums. Addition of the suspension of supported alkali metal to a solution of zinc chloride gave an active zinc on polymeric support, which can be used for the Reformatski and Barbier reactions.
- Majkosza, Mieczyslaw,Nieczypor, Piotr,Grela, Karol
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p. 10827 - 10836
(2007/10/03)
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- Ambident Reactivity of Medium-Ring Cycloalkane-1,3-dione Enolates
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Cycloalkane-1,3-diones with ring sizes 7-10 have been converted to their enolates and subjected to a variety of ethylation and methylation reagent/solvent systems. The greatest amount of O-alkylation was encountered using ethyl tosylate in HMPA. The O/C alkylation ratios decreased with almost every reagent/solvent system as the ring size was increased. This trend is consistent with greater steric strain in the conjugated enolate resonance contributor, resulting in diminished O-attack as the ring size is increased.
- Thompson, Glenn S.,Hirsch, Jerry A.
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p. 1098 - 1101
(2007/10/03)
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- Convenient Preparation of 'High-Surface Sodium' in Liquid Ammonia: Use in the Acyloin Reaction
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'Sodium on solid support' (5-20 wt.% of Na on NaCl, glass powder, poly(ethylene) and poly(propylene)) can be conveniently prepared via low-temperature (-33°C) deposition of sodium from its solution in liquid ammonia. Use of this reagent in the acyloin reaction of carboxylic esters gave the corresponding products in good yields.
- Makosza, Mieczyslaw,Grela, Karol
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p. 267 - 268
(2007/10/03)
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- Cascade reactions of methyl-2-chloro-2-cyclopropylideneacetate with five- and seven-membered cyclic dienolates: A novel approach to the bicyclo[4.2.1]nonane segment of the skeleton of mediterraneols
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The MIMIRC (Michael-Michael-Ring Closure) reaction of methyl 2-chloro-2-cyclopropylideneacetate (5) with the cyclic dienolates 6a, 6c, and the one derived from 11-R under aprotic conditions gave the tricyclic adducts 7a, 7c, and 10-R, respectively, in moderate to good yield. Compound 10-R is conceived as a potential intermediate for the synthesis of the biologically active marine diterpenes mediterraneol 1.
- Hadjiarapoglou,Klein,Spitzner,De Meijere
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p. 525 - 528
(2007/10/03)
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- Radical tandem cyclizations by anodic decarboxylation of carboxylic acids
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Radical tandem cyclizations are initiated by the Kolbe electrolysis of unsaturated carboxylic acids 4, 18, 23-25 which are prepared in a few steps. The efficiency of the radical tandem cyclization provides a short synthetic sequence to tricyclic products, e.g. angular triquinanes 7, 8, 11, 26-28. In this anodic tandem cyclization, three C-C bonds are formed regio- and stereoselectively in a one-pot reaction by intramolecular addition and intermolecular coupling. The use of different carboxylic acids as starting materials and various coacids gives versatile access to substituted tricyclic compounds.
- Matzeit,Schafer,Amatore
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p. 1432 - 1444
(2007/10/02)
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- Efficient Preparation of Cis Vicinal Tertiary Diamines from 2-Hydroxy Ketones in Two Steps
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Cyclic (C5 and C6) cis vicinal tertiary diamines are efficiently prepared by catalytic hydrogenation, Pd(C), of the corresponding N-substituted amino enamines, e.g. 6.The latter are obtained by p-toluenesulfonic acid catalyzed condensation of secondary amines with cyclic 2-hydroxy ketones in refluxing benzene under Dean-Stark conditions or from the N-substituted 2-amino ketones.For example cis-1,2-dipyrrolidinocyclohexane has been obtained from adipoin in 69percent overall yield, isolated.
- Fraenkel, Gideon,Gallucci, Judith,Rosenzweig, Howard S.
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p. 677 - 681
(2007/10/02)
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