C07F7/1892

A PROCESS FOR THE PRODUCTION OF SULFUR CONTAINING SILANES BY UTILIZATION OF PHASE TRANSFER CATALYSIS

The invention relates to a process for the production of sulfur containing silanes by the following steps (a) preparing an aqueous phase preparation by mixing sodium hydrosulfide or sodium sulfide, sulfur, Na2C03 and/or NaOH and a brine of step (f) and optionally of aqueous suspension of step (h), (b) adding 20 - 100 wt. -% of the total amount of phase transfer catalyst (c) continuously or in portions adding halogen alkyl silane, and simultaneously adding the rest of the total amount of phase transfer catalyst, in portions or continuously, (d) optionally adding brine from (f), optionally adding aqueous suspension from (h), optionally adding solid residue from step (k), separate the phase into a lower aqueous suspension and an upper organic phase and draw off the organic phase, (e) supply of the aqueous suspension from (d), optionally adding aqueous suspension from (h), separate in a salt cake and brine, (f) recycle all or a part of the brine of step (e) into step (a) and optional into step (d), (g) optionally distillate the rest of the brine from step (e) to yield aqueous distillate and aqueous suspension, (h) optionally recycle the aqueous suspension of step (g) into step (a) and /or (d) and/ or (e), (i) route the organic phase of step (d) to an evaporation step to yield a organic residue and low boiling distillate, (j) separate the organic residue from the evaporation step (i) into a sulfur containing silane and a solid residue, (k) optionally the solid residue of step (j) is recycled to step (d).

Silanes and Curable Compositions Containing Said Silanes as Crosslinkers
20180002353 · 2018-01-04 ·

The invention relates to a silane of the formula (1),


Si(R.sup.1).sub.m(R.sup.2).sub.n(R.sup.3).sub.4-(m+n)  (1)

as defined herein, where the silane has at least one group of the general formula (3):

##STR00001##

as defined herein, to a method for preparing the silane, and to curable compositions, containing the silane and at least one polyorganosiloxane.

PROCESSES AND INTERMEDIATES FOR THE PREPARATIONS OF BENZOPROSTACYCLIN ANALOGUES AND BENZOPROSTACYCLIN ANALOGUES PREPARED THEREFROM

The invention relates to processes for preparing benzoprostacyclin analogues and intermediates prepared from the process, and the benzoprostacyclin analogues prepared therefrom. The invention also relates to cyclopentenone intermediates in racemic or optically active form.

Intermediates useful in the preparation of halichondrin compounds and methods for preparing the same

The invention relates to intermediates useful in the preparation of halichondrin compounds, methods for preparing the same and use thereof, such as halichondrins, eribulin, or their analogs. The intermediates, the methods and use thereof are used for the synthesis of the C20-C26 fragment of halichondrin compounds. The raw materials in the synthetic route of the invention are cheap and easily obtained, the sources and the qualities of the raw materials are reliable. The choice of the methods useful in the synthesis of chiral central structures are based on the structural characteristics of the reactants, thus effectively improving the synthesis efficiency, reducing the difficulties and risks of product quality control, and avoiding the use of highly toxic and expensive organotin catalysts to significantly decrease costs and improve environmental friendliness.

VISIBLE-LIGHT MEDIATED ORGANOPHOTOREDOX CATALYTIC DEUTERATION OF AROMATIC AND ALIPHATIC ALDEHYDES
20230016922 · 2023-01-19 ·

Described are methods for preparing a deuterated aldehyde using with a photocatalyst and a hydrogen atom transfer agent in a H.sub.2O free solvent comprising D.sub.2O and an organic solvent under an inert gas. The methods may be used to convert a wide variety of aldehydes (e.g., aryl, alkyl, or alkenyl aldehydes) to C-1 deuterated aldehydes under mild reaction conditions.

Process for preparing polysulfane silanes

Process for preparing polysulfane silanes of the formula I
(R.sup.1O).sub.3-mR.sup.2.sub.mSi—R.sup.3—S.sub.x—R.sup.3—SiR.sup.2.sub.m(OR.sup.1).sub.3-m  I,
by reaction of silane of the formula II
(R.sup.1O).sub.3-mR.sup.2.sub.mSi—R.sup.3-Hal  II,
with one or more metal sulfides of the formula III
Me(SH).sub.f and/or Me.sub.3-fS.sub.x-y  III,
optionally in the presence of one or more salts of monohydric or polyhydric acids,
with the optional addition of y mol of sulfur in aqueous R.sup.1—OH solution, wherein the water content of the aqueous R.sup.1—OH solution is 5% to 40% by weight,
wherein a. the process stream from the reaction of silane of the formula II with one or more metal sulfides of the formula III, optionally in the presence of one or more salts and optionally with the addition of sulfur, in aqueous R.sup.1—OH solution, comprising polysulfane silanes of the formula I, silane of the formula II, metal sulfides of the formula III, solvent R.sup.1—OH, water and process salts,
is combined with the wash solution from step d, comprising solvent R.sup.1—OH, water and polysulfane silanes of the formula I, b. the solvent R.sup.1—OH and water are removed by distillation, c. the remaining suspension comprising polysulfane silane of the formula I and process salt is subjected to a filtration or a sedimentation and d. the process salt from step c is washed with solvent R.sup.1—OH and then dried, the wash solution comprising solvent R.sup.1—OH, water and polysulfane silane of the formula I is recycled to process step a.

Method for producing iodine-containing silicon compound

A method for producing a silicon compound containing an iodophenyl group, including substituting iodine for a trialkylsilyl ((R.sup.0).sub.3Si) group bonded to a phenyl group by using an iodine-containing electrophilic reagent (I-X) as shown by the following reaction equation: ##STR00001##
where all of R.sup.0's may be identical to or different from each other and each represent an alkyl group having 1 to 6 carbon atoms; R.sup.1 represents a single bond or a divalent organic group; R.sup.2 represents an organic group having 1 to 10 carbon atoms; R.sup.3 represents an organic group having 1 to 10 carbon atoms; R represents an organic group having 1 to 6 carbon atoms; n0 is 1, 2, or 3, n1 is 1, 2, or 3, n2 is 0, 1, or 2, and n3 is 0, 1, or 2, provided that 1≤n1+n3≤3; and X represents a counter substituent of iodine, acting as an electrophilic reactive species.

Benzyl compound

The purpose of the present invention is to provide a protecting group which improves the solubility of a compound having a functional group protected with the protecting group in an organic solvent and which is easily separated and purified after a reaction with avoiding solidification or insolubilization. Provided is a benzyl compound represented by Formula (1) where X.sup.1 represents —CH.sub.2OR.sup.14 (where R.sup.14 represents a hydrogen atom, a halogenocarbonyl group, or an active ester-type protecting group), —CH.sub.2NHR.sup.5 (where R.sup.15 represents a hydrogen atom, a linear or branched alkyl group having 1 to 6 carbon atoms, or an aralkyl group), a halogenomethyl group, a methyl azide group, a formyl group, or an oxime; and at least one of R.sup.1, R.sup.2, R.sup.3, R.sup.4, and R.sup.5 is a group represented by Formula (2), and the remainders each represent a hydrogen atom, a halogen atom, an alkyl group having 1 to 4 carbon atoms, or an alkoxy group having 1 to 4 carbon atoms, where R.sup.6 represents a linear or branched alkylene group having 1 to 16 carbon atoms; X.sup.2 represents O or CONR.sup.16 (where R.sup.16 represents a hydrogen atom or an alkyl group having 1 to 4 carbon atoms); and A represents a group represented by Formula (3), (4), (5), (6), (7), (8), (9), (10), (11), (12), or (13).

Process and intermediates for the preparation of eldecalcitol

The invention relates to new intermediates in the synthesis of Eldecalcitol and to processes for the preparation of said intermediates and of Eldecalcitol.

Tertiary Hydroxyl Functional Alkoxysilanes and Methods for Preparing Thereof
20220363699 · 2022-11-17 ·

Disclosed is a tertiary hydroxyl functional alkoxysilane of the general formula (I)

##STR00001##

wherein R.sup.1 is selected from the group consisting of hydrogen and a linear or branched, substituted or unsubstituted hydrocarbon residue having 1 to 20 carbon atoms; R.sup.2 and R.sup.3 are same or different and are, independent from one another, selected from a linear or branched, substituted or unsubstituted hydrocarbon residue having 1 to 20 carbon atoms; R.sup.4 is selected from a linear or branched, substituted or unsubstituted hydrocarbon residue having 1 to 20 carbon atoms; R.sup.5 is selected from a linear or branched, substituted or unsubstituted hydrocarbon residue having 1 to 20 carbon atoms; R.sup.6 and R.sup.7 are same or different and are, independent from one another, selected from a linear or branched, substituted or unsubstituted hydrocarbon residue having 1 to 20 carbon atoms; and n is 1, 2 or 3, a method for preparing thereof, and the use of the tertiary hydroxyl functional alkoxysilane of the general formula (I).